Poly[μ(3)-acetato-di-μ(3)-isonicotinato-μ(2)-isonicotinato-samarium(III)silver(I)].

In the title homochiral three-dimensional heterometallic complex, [AgSm(C(6)H(4)NO(2))(3)(C(2)H(3)O(2))](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 tetra-hedral 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 = 683.58

Hexagonal,

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[F 2 > 2σ(F 2)] = 0.020

wR(F 2) = 0.049

S = 1.06

1992 reflections

154 parameters

H-atom parameters constrained

Δρmax = 0.65 e Å−3

Δρmin = −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.

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

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

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[AgSm(C6H4NO2)3(C2H3O2)]	Dx = 2.059 Mg m−3
Mr = 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

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

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(Fo2) + (0.0242P)2 + 2.1731P] where P = (Fo2 + 2Fc2)/3
S = 1.06	(Δ/σ)max = 0.001
1992 reflections	Δρmax = 0.65 e Å−3
154 parameters	Δρmin = −0.45 e Å−3
0 restraints	Absolute structure: Flack (1983), 739 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.006 (15)

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.

	x	y	z	Uiso*/Ueq	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)

	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)

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—O1iv	2.478 (3)	C5—C6	1.386 (7)
Sm1—O1v	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—N1vi	2.316 (4)	C8—H11A	0.9600
Ag2—O3	2.328 (3)	C8—H11B	0.9600
Ag2—O3vi	2.328 (3)	C8—H11C	0.9600
O1—C1	1.248 (5)	C9—O4vi	1.238 (4)
O1—Sm1vii	2.478 (3)	C9—C10	1.521 (8)
O2—C1	1.261 (5)	C10—C11	1.376 (6)
O2—Sm1viii	2.336 (3)	C10—C11vi	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—C12vi	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—O1iv	102.15 (10)	C3—C2—C1	122.4 (4)
O2ii—Sm1—O1iv	83.83 (10)	C4—C3—C2	119.2 (4)
O4—Sm1—O1iv	145.28 (11)	C4—C3—H4	120.4
O4iii—Sm1—O1iv	73.30 (11)	C2—C3—H4	120.4
O2i—Sm1—O1v	83.83 (10)	N1—C4—C3	124.3 (4)
O2ii—Sm1—O1v	102.15 (10)	N1—C4—H2	117.9
O4—Sm1—O1v	73.30 (11)	C3—C4—H2	117.9
O4iii—Sm1—O1v	145.28 (11)	N1—C5—C6	123.5 (5)
O1iv—Sm1—O1v	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
O1iv—Sm1—O3	72.14 (10)	O3iii—C7—O3	118.3 (5)
O1v—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)
O1iv—Sm1—O3iii	72.89 (11)	C7—C8—H11A	109.5
O1v—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—O4vi	127.5 (6)
O1iv—Sm1—C7	70.51 (8)	O4—C9—C10	116.3 (3)
O1v—Sm1—C7	70.51 (8)	O4vi—C9—C10	116.3 (3)
O3—Sm1—C7	25.76 (7)	C11—C10—C11vi	117.6 (6)
O3iii—Sm1—C7	25.76 (7)	C11—C10—C9	121.2 (3)
N1—Ag2—N1vi	102.7 (2)	C11vi—C10—C9	121.2 (3)
N1—Ag2—O3	105.05 (13)	C10—C11—C12	118.8 (5)
N1vi—Ag2—O3	112.42 (14)	C10—C11—H13	120.6
N1—Ag2—O3vi	112.42 (14)	C12—C11—H13	120.6
N1vi—Ag2—O3vi	105.05 (13)	N2—C12—C11	125.0 (6)
O3—Ag2—O3vi	118.21 (15)	N2—C12—H14	117.5
C1—O1—Sm1vii	124.3 (3)	C11—C12—H14	117.5
C1—O2—Sm1viii	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—C12vi	114.9 (7)