Poly[bis-(N,N-dimethyl-formamide)tris-(μ(4)-trans-stilbene-4,4'-dicarboxyl-ato)-tricadmium(II)]: a two-dimensional network with an unusual 3 topology.

In the title compound, [Cd(3)(C(16)H(10)O(4))(3)(C(3)H(7)NO)(2)](n) or [Cd(3)(SDA)(3)(DMF)(2)](n) (H(2)SDA is trans-stilbene-4,4'-dicarboxylic acid and DMF is dimethyl-formamide), the linear dicarboxylate ligand forms a two-dimensionally layered metal-organic network with the relatively uncommon 3(6) topology. The structure reveals trinuclear secondary building units and has an octa-hedral geometry at a central metal ion (occupying a symmetry site) and tetra-hedral geometries at two surrounding symmetrically equivalent metal ions lying on a threefold axis. The six-connected planar trinuclear Cd(II) centers, Cd(3)(O(2)CR)(6), play a role as potential nodes in generation of the relatively uncommon 3(6) topology. The coordinated DMF unit is disordered around the threefold axis.

Related literature

For related literature, see: Chi et al. (2006 ▶); Dincâ & Long (2005 ▶); Dybtsev et al. (2004 ▶); Eddaoudi et al. (2002 ▶); Edgar et al. (2001 ▶); Hawxwell et al. (2006 ▶); Hill et al. (2005 ▶); Luan et al. (2006 ▶); Park et al. (2006 ▶); Rosi et al. (2003 ▶); Saalfrank et al. (2001 ▶); Seo et al. (2000 ▶); Wang et al. (2006 ▶); Williams et al. (2005 ▶).

Experimental

Crystal data

[Cd3(C16H10O4)3(C3H7NO)2]

M = 1282.11

Trigonal,

a = 16.4881 (5) Å

c = 16.7919 (10) Å

V = 3953.4 (3) Å3

Z = 3

Mo Kα radiation

μ = 1.27 mm−1

T = 223 (2) K

0.30 × 0.30 × 0.30 mm

Data collection

Bruker SMART CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.69, T max = 0.69

6604 measured reflections

2105 independent reflections

1782 reflections with I > 2σ(I)

R int = 0.104

Refinement

R[F 2 > 2σ(F 2)] = 0.057

wR(F 2) = 0.181

S = 1.18

2105 reflections

136 parameters

92 restraints

H-atom parameters constrained

Δρmax = 1.70 e Å−3

Δρmin = −1.53 e Å−3

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); 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 I, global. DOI: 10.1107/S1600536808016267/n class="CellLine">bg2189sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808016267/bg2189Isup2.hkl

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

[Cd3(C16H10O4)3(C3H7N1O1)2]	Z = 3
Mr = 1282.11	F000 = 1914
Trigonal, R3	Dx = 1.616 Mg m−3
Hall symbol: -R 3	Mo Kα radiation λ = 0.71073 Å
a = 16.4881 (5) Å	Cell parameters from 6604 reflections
b = 16.4881 (5) Å	θ = 1.9–28.4º
c = 16.7919 (10) Å	µ = 1.27 mm−1
α = 90º	T = 223 (2) K
β = 90º	Cubic, colourless
γ = 120º	0.30 × 0.30 × 0.30 mm
V = 3953.4 (3) Å3

Siemens SMART CCD diffractometer	2105 independent reflections
Radiation source: fine-focus sealed tube	1782 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.104
T = 223(2) K	θmax = 28.4º
ω scans	θmin = 1.9º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −21→21
Tmin = 0.69, Tmax = 0.69	k = −21→18
6604 measured reflections	l = −21→22

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)] = 0.057	H-atom parameters constrained
wR(F2) = 0.181	w = 1/[σ2(Fo2) + (0.0995P)2 + 4.8382P] where P = (Fo2 + 2Fc2)/3
S = 1.18	(Δ/σ)max = 0.001
2105 reflections	Δρmax = 1.70 e Å−3
136 parameters	Δρmin = −1.53 e Å−3
92 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

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)
Cd1	0.0000	1.0000	1.0000	0.0302 (2)
Cd2	0.0000	1.0000	0.79310 (3)	0.0424 (2)
O1	0.1245 (2)	1.0679 (2)	0.9162 (2)	0.0521 (7)
O2	0.1222 (2)	1.1401 (2)	0.8067 (2)	0.0599 (9)
C1	0.1562 (3)	1.1402 (3)	0.8740 (3)	0.0458 (9)
C2	0.2391 (3)	1.2283 (3)	0.9015 (3)	0.0579 (12)
C3	0.2624 (5)	1.3134 (4)	0.8665 (4)	0.0748 (17)
H3A	0.2259	1.3142	0.8238	0.090*
C4	0.3368 (6)	1.3965 (5)	0.8918 (5)	0.109 (3)
H4A	0.3496	1.4531	0.8677	0.131*
C5	0.3911 (6)	1.3967 (5)	0.9510 (5)	0.112 (3)
C6	0.4698 (8)	1.4929 (7)	0.9730 (7)	0.138 (4)
H6	0.4748	1.5449	0.9456	0.166*
C7	0.3714 (7)	1.3114 (7)	0.9864 (6)	0.133 (4)
H7A	0.4095	1.3120	1.0283	0.159*
C8	0.2968 (5)	1.2260 (5)	0.9610 (4)	0.099 (3)
H8A	0.2859	1.1690	0.9831	0.118*
O1S	0.0000	1.0000	0.6625 (11)	0.186 (4)
N1S	0.106 (2)	1.082 (2)	0.5571 (18)	0.188 (5)	0.33
C1S	0.067 (4)	1.086 (4)	0.625 (2)	0.190 (6)	0.33
H1S	0.0825	1.1436	0.6479	0.228*	0.33
C2S	0.136 (3)	1.014 (3)	0.547 (3)	0.188 (5)	0.33
H2S1	0.1426	0.9916	0.5985	0.282*	0.33
H2S2	0.1958	1.0429	0.5194	0.282*	0.33
H2S3	0.0899	0.9616	0.5156	0.282*	0.33
C3S	0.144 (3)	1.160 (3)	0.502 (2)	0.190 (5)	0.33
H3S1	0.0964	1.1771	0.4909	0.284*	0.33
H3S2	0.1615	1.1420	0.4531	0.284*	0.33
H3S3	0.1980	1.2129	0.5257	0.284*	0.33

	U11	U22	U33	U12	U13	U23
Cd1	0.0307 (3)	0.0307 (3)	0.0291 (4)	0.01536 (14)	0.000	0.000
Cd2	0.0414 (3)	0.0414 (3)	0.0443 (4)	0.02070 (14)	0.000	0.000
O1	0.0407 (15)	0.0402 (15)	0.068 (2)	0.0147 (13)	0.0172 (14)	0.0081 (13)
O2	0.0493 (17)	0.061 (2)	0.0463 (17)	0.0106 (15)	0.0029 (13)	0.0043 (14)
C1	0.0361 (19)	0.044 (2)	0.047 (2)	0.0117 (16)	0.0112 (16)	0.0003 (16)
C2	0.052 (3)	0.048 (2)	0.048 (2)	0.006 (2)	0.0016 (19)	0.0048 (18)
C3	0.062 (3)	0.047 (3)	0.090 (4)	0.008 (3)	−0.004 (3)	0.013 (3)
C4	0.093 (5)	0.045 (3)	0.134 (7)	−0.006 (3)	−0.026 (5)	0.008 (4)
C5	0.108 (6)	0.067 (4)	0.091 (5)	−0.008 (4)	−0.016 (4)	−0.006 (4)
C6	0.137 (8)	0.095 (6)	0.130 (8)	0.018 (5)	−0.037 (6)	0.024 (5)
C7	0.113 (7)	0.112 (7)	0.094 (5)	−0.003 (5)	−0.057 (5)	0.013 (5)
C8	0.090 (4)	0.075 (4)	0.075 (4)	−0.001 (3)	−0.032 (3)	0.025 (3)
O1S	0.192 (4)	0.192 (4)	0.174 (6)	0.096 (2)	0.000	0.000
N1S	0.186 (6)	0.190 (6)	0.181 (6)	0.089 (4)	0.000 (4)	0.000 (4)
C1S	0.192 (8)	0.191 (7)	0.178 (7)	0.088 (6)	−0.002 (5)	−0.006 (5)
C2S	0.186 (6)	0.190 (6)	0.183 (6)	0.090 (4)	−0.001 (4)	0.001 (4)
C3S	0.189 (6)	0.190 (6)	0.184 (6)	0.090 (4)	0.000 (4)	0.001 (4)

Cd1—O1i	2.269 (3)	C5—C7	1.408 (13)
Cd1—O1ii	2.269 (3)	C5—C6	1.509 (12)
Cd1—O1iii	2.269 (3)	C6—C6vi	1.279 (19)
Cd1—O1	2.269 (3)	C6—H6	0.9400
Cd1—O1iv	2.269 (3)	C7—C8	1.395 (10)
Cd1—O1v	2.269 (3)	C7—H7A	0.9400
Cd1—Cd2v	3.4742 (5)	C8—H8A	0.9400
Cd1—Cd2	3.4742 (5)	O1S—C1Siii	1.43 (4)
Cd2—O2	2.189 (3)	O1S—C1Si	1.43 (4)
Cd2—O2iii	2.189 (3)	O1S—C1S	1.43 (4)
Cd2—O2i	2.189 (3)	N1S—C1S	1.323 (9)
Cd2—O1S	2.193 (19)	N1S—C3S	1.445 (9)
O1—C1	1.255 (5)	N1S—C2S	1.448 (9)
O2—C1	1.262 (6)	C1S—H1S	0.9400
C1—C2	1.484 (6)	C2S—H2S1	0.9700
C2—C3	1.386 (8)	C2S—H2S2	0.9700
C2—C8	1.394 (8)	C2S—H2S3	0.9700
C3—C4	1.373 (9)	C3S—H3S1	0.9700
C3—H3A	0.9400	C3S—H3S2	0.9700
C4—C5	1.336 (12)	C3S—H3S3	0.9700
C4—H4A	0.9400
O1i—Cd1—O1ii	180.00 (13)	C3—C2—C1	120.9 (5)
O1i—Cd1—O1iii	85.62 (14)	C8—C2—C1	120.1 (5)
O1ii—Cd1—O1iii	94.38 (14)	C4—C3—C2	122.4 (7)
O1i—Cd1—O1	85.62 (14)	C4—C3—H3A	118.8
O1ii—Cd1—O1	94.38 (14)	C2—C3—H3A	118.8
O1iii—Cd1—O1	85.62 (14)	C5—C4—C3	119.8 (7)
O1i—Cd1—O1iv	94.38 (14)	C5—C4—H4A	120.1
O1ii—Cd1—O1iv	85.62 (14)	C3—C4—H4A	120.1
O1iii—Cd1—O1iv	180.000 (1)	C4—C5—C7	119.5 (6)
O1—Cd1—O1iv	94.38 (14)	C4—C5—C6	114.1 (8)
O1i—Cd1—O1v	94.38 (14)	C7—C5—C6	126.4 (8)
O1ii—Cd1—O1v	85.62 (14)	C6vi—C6—C5	123.3 (13)
O1iii—Cd1—O1v	94.38 (14)	C6vi—C6—H6	118.4
O1—Cd1—O1v	180.000 (1)	C5—C6—H6	118.4
O1iv—Cd1—O1v	85.62 (14)	C8—C7—C5	121.7 (7)
O1i—Cd1—Cd2v	128.30 (9)	C8—C7—H7A	119.1
O1ii—Cd1—Cd2v	51.70 (9)	C5—C7—H7A	119.1
O1iii—Cd1—Cd2v	128.30 (9)	C7—C8—C2	117.4 (7)
O1—Cd1—Cd2v	128.30 (9)	C7—C8—H8A	121.3
O1iv—Cd1—Cd2v	51.70 (9)	C2—C8—H8A	121.3
O1v—Cd1—Cd2v	51.70 (9)	C1Siii—O1S—C1Si	102 (3)
O1i—Cd1—Cd2	51.70 (9)	C1Siii—O1S—C1S	102 (3)
O1ii—Cd1—Cd2	128.30 (9)	C1Si—O1S—C1S	102 (3)
O1iii—Cd1—Cd2	51.70 (9)	C1Siii—O1S—Cd2	116 (2)
O1—Cd1—Cd2	51.70 (9)	C1Si—O1S—Cd2	116 (2)
O1iv—Cd1—Cd2	128.30 (9)	C1S—O1S—Cd2	116 (2)
O1v—Cd1—Cd2	128.30 (9)	C1S—N1S—C3S	120.7 (11)
Cd2v—Cd1—Cd2	180.0	C1S—N1S—C2S	120.1 (11)
O2—Cd2—O2iii	118.93 (3)	C3S—N1S—C2S	116.8 (10)
O2—Cd2—O2i	118.93 (3)	N1S—C1S—O1S	119 (4)
O2iii—Cd2—O2i	118.93 (3)	N1S—C1S—H1S	120.4
O2—Cd2—O1S	95.98 (9)	O1S—C1S—H1S	120.4
O2iii—Cd2—O1S	95.98 (9)	N1S—C2S—H2S1	109.5
O2i—Cd2—O1S	95.98 (9)	N1S—C2S—H2S2	109.5
O2—Cd2—Cd1	84.02 (9)	H2S1—C2S—H2S2	109.5
O2iii—Cd2—Cd1	84.02 (9)	N1S—C2S—H2S3	109.5
O2i—Cd2—Cd1	84.02 (9)	H2S1—C2S—H2S3	109.5
O1S—Cd2—Cd1	180.000 (4)	H2S2—C2S—H2S3	109.5
C1—O1—Cd1	131.5 (3)	N1S—C3S—H3S1	109.5
C1—O2—Cd2	105.6 (3)	N1S—C3S—H3S2	109.5
O1—C1—O2	122.1 (4)	H3S1—C3S—H3S2	109.5
O1—C1—C2	119.8 (4)	N1S—C3S—H3S3	109.5
O2—C1—C2	118.1 (4)	H3S1—C3S—H3S3	109.5
C3—C2—C8	119.0 (5)	H3S2—C3S—H3S3	109.5