[μ-N,N,N',N'-Tetra-kis(2-pyridyl-meth-yl)butane-1,4-diamine]-bis-[dinitratocadmium(II)].

The title dinuclear cadmium complex, [Cd(2)(NO(3))(4)(C(28)H(32)N(6))], is located on an inversion center. The unique Cd(II) ion displays a 5 + 2 coordination. A distorted square-pyramidal geometry is formed by the dipicolyl-amine group of the ligand via the N atoms in a meridional fashion and two O atoms of the nitrate ligands with short Cd-O distances. The coordination is completed by two loosely bound O atoms of the nitrate ligands.

Related literature

For crystallographic data of tetra­kis­(pyridin-2-yl-meth­yl)alkyl-diamine compounds, see: Fujihara et al. (2004 ▶); Mambanda et al. (2007 ▶). For the superoxide dismutase activity of iron complexes, see: Tamura et al. (2000 ▶). For dinuclear Pt complexes of similar ligands, see: Ertürk et al. (2007 ▶). For the use of the dipicolyl­amine moiety for binding of the M(CO)3 core (M = Re, 99Tc), see: Bartholomä et al. (2009 ▶). For crystal structures closely related to the title compound, see: Bartholomä et al. (2010a ▶,b ▶,c ▶,d ▶)

Experimental

Crystal data

[Cd2(NO3)4(C28H32N6)]

M = 925.44

Triclinic,

a = 8.0548 (8) Å

b = 8.7010 (8) Å

c = 13.2566 (13) Å

α = 107.488 (2)°

β = 96.767 (2)°

γ = 104.631 (2)°

V = 838.30 (14) Å3

Z = 1

Mo Kα radiation

μ = 1.35 mm−1

T = 90 K

0.48 × 0.30 × 0.08 mm

Data collection

Bruker SMART APEX diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 1998 ▶) T min = 0.564, T max = 0.900

8382 measured reflections

4043 independent reflections

3912 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.030

wR(F 2) = 0.069

S = 1.15

4043 reflections

235 parameters

H-atom parameters constrained

Δρmax = 1.01 e Å−3

Δρmin = −0.50 e Å−3

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 1999 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810034549/lh5105sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810034549/lh5105Isup2.hkl

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

[Cd2(NO3)4(C28H32N6)]	Z = 1
Mr = 925.44	F(000) = 462
Triclinic, P1	Dx = 1.833 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.0548 (8) Å	Cell parameters from 5752 reflections
b = 8.7010 (8) Å	θ = 2.5–28.4°
c = 13.2566 (13) Å	µ = 1.35 mm−1
α = 107.488 (2)°	T = 90 K
β = 96.767 (2)°	Plate, colourless
γ = 104.631 (2)°	0.48 × 0.30 × 0.08 mm
V = 838.30 (14) Å3

Bruker SMART APEX diffractometer	4043 independent reflections
Radiation source: fine-focus sealed tube	3912 reflections with I > 2σ(I)
graphite	Rint = 0.020
Detector resolution: 512 pixels mm-1	θmax = 28.1°, θmin = 1.7°
φ and ω scans	h = −10→10
Absorption correction: multi-scan (SADABS; Bruker, 1998)	k = −11→11
Tmin = 0.564, Tmax = 0.900	l = −16→17
8382 measured reflections

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)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069	H-atom parameters constrained
S = 1.15	w = 1/[σ2(Fo2) + (0.0286P)2 + 0.8284P] where P = (Fo2 + 2Fc2)/3
4043 reflections	(Δ/σ)max = 0.001
235 parameters	Δρmax = 1.01 e Å−3
0 restraints	Δρmin = −0.50 e Å−3

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
Cd1	0.37059 (2)	0.85996 (2)	0.212593 (14)	0.01675 (6)
O1	0.4785 (3)	0.7640 (3)	0.05839 (16)	0.0335 (5)
O2	0.2104 (3)	0.6092 (3)	0.03615 (16)	0.0270 (4)
O3	0.3515 (3)	0.5592 (3)	−0.09358 (19)	0.0511 (7)
O4	0.5248 (3)	1.1197 (3)	0.39807 (18)	0.0347 (5)
O5	0.6551 (3)	1.0276 (3)	0.27055 (17)	0.0347 (5)
O6	0.7985 (3)	1.2505 (3)	0.41010 (18)	0.0356 (5)
N1	0.0990 (3)	0.8167 (2)	0.27756 (16)	0.0158 (4)
N2	0.2297 (3)	1.0238 (3)	0.15892 (16)	0.0186 (4)
N3	0.3643 (3)	0.6590 (3)	0.28768 (16)	0.0189 (4)
N4	0.3458 (3)	0.6419 (3)	−0.00139 (19)	0.0269 (5)
N5	0.6610 (3)	1.1361 (3)	0.36162 (18)	0.0221 (4)
C1	0.0530 (3)	0.6391 (3)	0.2732 (2)	0.0207 (5)
H1A	−0.0030	0.5639	0.1979	0.025*
H1B	−0.0335	0.6213	0.3190	0.025*
C2	0.2108 (3)	0.5907 (3)	0.31117 (19)	0.0194 (5)
C3	0.1947 (4)	0.4684 (3)	0.3606 (2)	0.0245 (5)
H3A	0.0869	0.4226	0.3787	0.029*
C4	0.3379 (4)	0.4149 (3)	0.3827 (2)	0.0276 (6)
H4A	0.3289	0.3310	0.4158	0.033*
C5	0.4951 (4)	0.4839 (3)	0.3566 (2)	0.0273 (6)
H5	0.5944	0.4475	0.3706	0.033*
C6	0.5034 (4)	0.6068 (3)	0.3099 (2)	0.0238 (5)
H6A	0.6109	0.6562	0.2928	0.029*
C7	−0.0241 (3)	0.8446 (3)	0.19778 (19)	0.0192 (5)
H7A	−0.1265	0.8629	0.2287	0.023*
H7B	−0.0672	0.7419	0.1322	0.023*
C8	0.0606 (3)	0.9957 (3)	0.16622 (18)	0.0175 (5)
C9	−0.0369 (3)	1.0924 (3)	0.13757 (19)	0.0203 (5)
H9	−0.1557	1.0729	0.1446	0.024*
C10	0.0413 (4)	1.2182 (3)	0.0984 (2)	0.0229 (5)
H10	−0.0244	1.2841	0.0772	0.028*
C11	0.2153 (4)	1.2464 (3)	0.0906 (2)	0.0225 (5)
H11	0.2712	1.3318	0.0641	0.027*
C12	0.3059 (3)	1.1477 (3)	0.1222 (2)	0.0208 (5)
H12	0.4260	1.1675	0.1180	0.025*
C13	0.1306 (3)	0.9396 (3)	0.38864 (18)	0.0167 (4)
H13A	0.1702	1.0550	0.3854	0.020*
H13B	0.2283	0.9253	0.4341	0.020*
C14	−0.0244 (3)	0.9281 (3)	0.44558 (19)	0.0194 (5)
H14A	−0.1265	0.9347	0.3994	0.023*
H14B	−0.0579	0.8180	0.4571	0.023*

	U11	U22	U33	U12	U13	U23
Cd1	0.01544 (9)	0.01864 (10)	0.01966 (10)	0.00647 (6)	0.00744 (6)	0.00900 (7)
O1	0.0278 (10)	0.0318 (11)	0.0282 (10)	−0.0031 (8)	0.0117 (8)	0.0001 (8)
O2	0.0228 (9)	0.0307 (10)	0.0304 (10)	0.0077 (8)	0.0088 (8)	0.0137 (8)
O3	0.0489 (14)	0.0507 (15)	0.0297 (12)	−0.0048 (12)	0.0180 (10)	−0.0073 (10)
O4	0.0253 (10)	0.0371 (11)	0.0373 (11)	0.0056 (9)	0.0163 (9)	0.0063 (9)
O5	0.0217 (10)	0.0412 (12)	0.0302 (11)	0.0043 (9)	0.0097 (8)	−0.0004 (9)
O6	0.0222 (10)	0.0322 (11)	0.0377 (12)	−0.0033 (8)	0.0008 (8)	0.0031 (9)
N1	0.0168 (9)	0.0142 (9)	0.0159 (9)	0.0048 (7)	0.0058 (7)	0.0036 (7)
N2	0.0203 (10)	0.0182 (10)	0.0184 (10)	0.0058 (8)	0.0056 (8)	0.0073 (8)
N3	0.0200 (10)	0.0176 (10)	0.0196 (10)	0.0061 (8)	0.0052 (8)	0.0063 (8)
N4	0.0271 (12)	0.0264 (11)	0.0255 (11)	0.0053 (9)	0.0100 (9)	0.0072 (9)
N5	0.0207 (10)	0.0242 (11)	0.0249 (11)	0.0093 (9)	0.0069 (8)	0.0105 (9)
C1	0.0185 (11)	0.0171 (11)	0.0258 (12)	0.0041 (9)	0.0082 (9)	0.0065 (9)
C2	0.0253 (12)	0.0146 (11)	0.0150 (11)	0.0036 (9)	0.0053 (9)	0.0018 (9)
C3	0.0313 (14)	0.0178 (12)	0.0194 (12)	0.0017 (10)	0.0049 (10)	0.0046 (9)
C4	0.0402 (16)	0.0172 (12)	0.0217 (12)	0.0043 (11)	−0.0005 (11)	0.0077 (10)
C5	0.0318 (14)	0.0210 (12)	0.0268 (13)	0.0094 (11)	−0.0017 (11)	0.0068 (10)
C6	0.0228 (12)	0.0215 (12)	0.0246 (12)	0.0059 (10)	0.0021 (10)	0.0062 (10)
C7	0.0161 (11)	0.0226 (12)	0.0180 (11)	0.0046 (9)	0.0046 (9)	0.0067 (9)
C8	0.0190 (11)	0.0190 (11)	0.0137 (10)	0.0065 (9)	0.0043 (8)	0.0035 (9)
C9	0.0194 (11)	0.0241 (12)	0.0181 (11)	0.0107 (9)	0.0047 (9)	0.0047 (9)
C10	0.0312 (14)	0.0218 (12)	0.0167 (11)	0.0142 (10)	0.0018 (10)	0.0039 (9)
C11	0.0302 (13)	0.0173 (11)	0.0192 (12)	0.0049 (10)	0.0045 (10)	0.0071 (9)
C12	0.0215 (12)	0.0201 (12)	0.0201 (12)	0.0040 (9)	0.0048 (9)	0.0078 (9)
C13	0.0159 (11)	0.0167 (10)	0.0152 (10)	0.0023 (8)	0.0048 (8)	0.0036 (8)
C14	0.0184 (11)	0.0199 (11)	0.0196 (12)	0.0059 (9)	0.0081 (9)	0.0047 (10)

Cd1—N2	2.250 (2)	C3—C4	1.381 (4)
Cd1—N3	2.251 (2)	C3—H3A	0.9500
Cd1—O5	2.279 (2)	C4—C5	1.389 (4)
Cd1—O1	2.322 (2)	C4—H4A	0.9500
Cd1—O2	2.588 (2)	C5—C6	1.379 (4)
Cd1—O4	2.687 (2)	C5—H5	0.9500
Cd1—N1	2.427 (2)	C6—H6A	0.9500
O1—N4	1.273 (3)	C7—C8	1.521 (3)
O2—N4	1.254 (3)	C7—H7A	0.9900
O3—N4	1.231 (3)	C7—H7B	0.9900
O4—N5	1.243 (3)	C8—C9	1.387 (3)
O5—N5	1.276 (3)	C9—C10	1.391 (4)
O6—N5	1.233 (3)	C9—H9	0.9500
N1—C1	1.477 (3)	C10—C11	1.382 (4)
N1—C7	1.479 (3)	C10—H10	0.9500
N1—C13	1.485 (3)	C11—C12	1.381 (4)
N2—C8	1.342 (3)	C11—H11	0.9500
N2—C12	1.351 (3)	C12—H12	0.9500
N3—C6	1.344 (3)	C13—C14	1.530 (3)
N3—C2	1.345 (3)	C13—H13A	0.9900
C1—C2	1.514 (4)	C13—H13B	0.9900
C1—H1A	0.9900	C14—C14i	1.528 (5)
C1—H1B	0.9900	C14—H14A	0.9900
C2—C3	1.396 (4)	C14—H14B	0.9900
N2—Cd1—N3	148.10 (8)	C3—C4—C5	119.9 (2)
N2—Cd1—O5	103.49 (8)	C3—C4—H4A	120.1
N3—Cd1—O5	103.16 (8)	C5—C4—H4A	120.1
N2—Cd1—O1	98.56 (8)	C6—C5—C4	118.3 (3)
N3—Cd1—O1	103.09 (8)	C6—C5—H5	120.9
O5—Cd1—O1	79.90 (7)	C4—C5—H5	120.9
N2—Cd1—N1	74.12 (7)	N3—C6—C5	122.2 (3)
N3—Cd1—N1	74.27 (7)	N3—C6—H6A	118.9
O5—Cd1—N1	139.43 (7)	C5—C6—H6A	118.9
O1—Cd1—N1	140.62 (7)	N1—C7—C8	112.38 (19)
N4—O1—Cd1	100.89 (15)	N1—C7—H7A	109.1
N5—O5—Cd1	105.38 (15)	C8—C7—H7A	109.1
C1—N1—C7	112.91 (19)	N1—C7—H7B	109.1
C1—N1—C13	113.20 (19)	C8—C7—H7B	109.1
C7—N1—C13	113.10 (19)	H7A—C7—H7B	107.9
C1—N1—Cd1	104.04 (14)	N2—C8—C9	121.2 (2)
C7—N1—Cd1	103.73 (14)	N2—C8—C7	117.4 (2)
C13—N1—Cd1	108.92 (13)	C9—C8—C7	121.2 (2)
C8—N2—C12	119.4 (2)	C8—C9—C10	119.3 (2)
C8—N2—Cd1	116.61 (16)	C8—C9—H9	120.4
C12—N2—Cd1	123.99 (17)	C10—C9—H9	120.4
C6—N3—C2	119.9 (2)	C11—C10—C9	119.4 (2)
C6—N3—Cd1	123.75 (17)	C11—C10—H10	120.3
C2—N3—Cd1	116.38 (17)	C9—C10—H10	120.3
O3—N4—O2	121.4 (2)	C12—C11—C10	118.4 (2)
O3—N4—O1	120.3 (2)	C12—C11—H11	120.8
O2—N4—O1	118.3 (2)	C10—C11—H11	120.8
O6—N5—O4	122.7 (2)	N2—C12—C11	122.3 (2)
O6—N5—O5	120.0 (2)	N2—C12—H12	118.8
O4—N5—O5	117.3 (2)	C11—C12—H12	118.8
N1—C1—C2	112.7 (2)	N1—C13—C14	116.85 (19)
N1—C1—H1A	109.0	N1—C13—H13A	108.1
C2—C1—H1A	109.0	C14—C13—H13A	108.1
N1—C1—H1B	109.0	N1—C13—H13B	108.1
C2—C1—H1B	109.0	C14—C13—H13B	108.1
H1A—C1—H1B	107.8	H13A—C13—H13B	107.3
N3—C2—C3	120.8 (2)	C14i—C14—C13	110.4 (2)
N3—C2—C1	117.8 (2)	C14i—C14—H14A	109.6
C3—C2—C1	121.2 (2)	C13—C14—H14A	109.6
C4—C3—C2	119.0 (3)	C14i—C14—H14B	109.6
C4—C3—H3A	120.5	C13—C14—H14B	109.6
C2—C3—H3A	120.5	H14A—C14—H14B	108.1
N2—Cd1—O1—N4	−82.99 (18)	Cd1—O5—N5—O6	−176.1 (2)
N3—Cd1—O1—N4	73.42 (18)	Cd1—O5—N5—O4	4.4 (3)
O5—Cd1—O1—N4	174.73 (19)	C7—N1—C1—C2	152.9 (2)
N1—Cd1—O1—N4	−7.6 (2)	C13—N1—C1—C2	−77.0 (3)
N2—Cd1—O5—N5	74.64 (18)	Cd1—N1—C1—C2	41.1 (2)
N3—Cd1—O5—N5	−87.67 (18)	C6—N3—C2—C3	1.3 (3)
O1—Cd1—O5—N5	171.11 (18)	Cd1—N3—C2—C3	−178.25 (17)
N1—Cd1—O5—N5	−6.6 (2)	C6—N3—C2—C1	−173.2 (2)
N2—Cd1—N1—C1	147.56 (15)	Cd1—N3—C2—C1	7.2 (3)
N3—Cd1—N1—C1	−28.13 (14)	N1—C1—C2—N3	−35.6 (3)
O5—Cd1—N1—C1	−120.12 (16)	N1—C1—C2—C3	149.8 (2)
O1—Cd1—N1—C1	63.46 (19)	N3—C2—C3—C4	−1.6 (4)
N2—Cd1—N1—C7	29.25 (14)	C1—C2—C3—C4	172.8 (2)
N3—Cd1—N1—C7	−146.43 (15)	C2—C3—C4—C5	0.6 (4)
O5—Cd1—N1—C7	121.57 (16)	C3—C4—C5—C6	0.7 (4)
O1—Cd1—N1—C7	−54.85 (19)	C2—N3—C6—C5	0.0 (4)
N2—Cd1—N1—C13	−91.45 (15)	Cd1—N3—C6—C5	179.57 (19)
N3—Cd1—N1—C13	92.86 (15)	C4—C5—C6—N3	−1.0 (4)
O5—Cd1—N1—C13	0.9 (2)	C1—N1—C7—C8	−154.2 (2)
O1—Cd1—N1—C13	−175.55 (14)	C13—N1—C7—C8	75.6 (2)
N3—Cd1—N2—C8	−5.2 (3)	Cd1—N1—C7—C8	−42.3 (2)
O5—Cd1—N2—C8	−151.19 (16)	C12—N2—C8—C9	−0.5 (3)
O1—Cd1—N2—C8	127.22 (17)	Cd1—N2—C8—C9	178.50 (17)
N1—Cd1—N2—C8	−13.12 (16)	C12—N2—C8—C7	174.4 (2)
N3—Cd1—N2—C12	173.73 (17)	Cd1—N2—C8—C7	−6.6 (3)
O5—Cd1—N2—C12	27.8 (2)	N1—C7—C8—N2	36.1 (3)
O1—Cd1—N2—C12	−53.8 (2)	N1—C7—C8—C9	−149.0 (2)
N1—Cd1—N2—C12	165.9 (2)	N2—C8—C9—C10	1.4 (4)
N2—Cd1—N3—C6	−175.28 (17)	C7—C8—C9—C10	−173.3 (2)
O5—Cd1—N3—C6	−29.3 (2)	C8—C9—C10—C11	−1.2 (4)
O1—Cd1—N3—C6	53.2 (2)	C9—C10—C11—C12	0.1 (4)
N1—Cd1—N3—C6	−167.4 (2)	C8—N2—C12—C11	−0.7 (4)
N2—Cd1—N3—C2	4.3 (3)	Cd1—N2—C12—C11	−179.60 (18)
O5—Cd1—N3—C2	150.30 (16)	C10—C11—C12—N2	0.9 (4)
O1—Cd1—N3—C2	−127.20 (17)	C1—N1—C13—C14	−62.6 (3)
N1—Cd1—N3—C2	12.17 (16)	C7—N1—C13—C14	67.4 (3)
Cd1—O1—N4—O3	178.6 (2)	Cd1—N1—C13—C14	−177.82 (17)
Cd1—O1—N4—O2	−1.2 (3)	N1—C13—C14—C14i	−175.1 (2)

Table 1

Selected bond lengths (Å)

Cd1—N2	2.250 (2)
Cd1—N3	2.251 (2)
Cd1—O5	2.279 (2)
Cd1—O1	2.322 (2)
Cd1—O2	2.588 (2)
Cd1—O4	2.687 (2)
Cd1—N1	2.427 (2)