catena-Poly[[bis-[[bis-(3-amino-prop-yl)amine-κN,N',N''](thio-cyanato-κN)cadmium]-μ(4)-sulfato-κO,O:O',O'] methanol hemisolvate].

The asymmetric unit of the title compound, {[Cd(2)(NCS)(2)(SO(4))(C(6)H(17)N(3))(2)]·0.5CH(3)OH}(n), consists of two Cd(2+) cations, two thio-cyanate and one sulfate anion, two bis-(3-amino-prop-yl)amine co-ligands and one methanol molecule with half-occupancy. Each Cd(2+) cation is coordinated by four N atoms of one terminal N-bonded thio-cyanate anion and one bis-(3-amino-prop-yl)amine co-ligand, and by two O atoms of two symmetry-related sulfate anions, defining a slightly distorted octa-hedral coordination polyhedron. Each two Cd(2+) cations are connected into dimers, which are located on centres of inversion and which are further μ-1,1:3,3-bridged via the sulfate anions into polymeric zigzag chains along the a axis.

Related literature

For background information about thermal decomposition reactions and the resulting inter­mediates, see: Boeckmann & Näther (2010 ▶, 2011 ▶); Boeckmann et al. (2011 ▶); Wöhlert et al. (2011 ▶); Wriedt et al. (2009a ▶,b ▶); Wriedt & Näther (2010 ▶).

Experimental

Crystal data

[Cd2(NCS)2(SO4)(C6H17N3)2]·0.5CH4O

M = 715.49

Triclinic,

a = 10.6648 (9) Å

b = 12.4441 (12) Å

c = 12.9240 (12) Å

α = 61.359 (10)°

β = 69.064 (10)°

γ = 68.772 (10)°

V = 1367.3 (2) Å3

Z = 2

Mo Kα radiation

μ = 1.82 mm−1

T = 200 K

0.18 × 0.13 × 0.09 mm

Data collection

STOE IPDS-1 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.746, T max = 0.841

12730 measured reflections

5736 independent reflections

4365 reflections with I > 2σ(I)

R int = 0.040

Refinement

R[F 2 > 2σ(F 2)] = 0.042

wR(F 2) = 0.113

S = 1.07

5736 reflections

301 parameters

H-atom parameters constrained

Δρmax = 1.07 e Å−3

Δρmin = −0.87 e Å−3

Data collection: X-AREA (Stoe & Cie, 2008 ▶); cell refinement: X-AREA; data reduction: X-AREA; 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 ▶) and DIAMOND (Brandenburg, 2011 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811031163/bt5596sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811031163/bt5596Isup2.hkl

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

[Cd2(NCS)2(SO4)(C6H17N3)2]·0.5CH4O	Z = 2
Mr = 715.49	F(000) = 718
Triclinic, P1	Dx = 1.738 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.6648 (9) Å	Cell parameters from 13797 reflections
b = 12.4441 (12) Å	θ = 2.5–27.0°
c = 12.9240 (12) Å	µ = 1.82 mm−1
α = 61.359 (10)°	T = 200 K
β = 69.064 (10)°	Block, colourless
γ = 68.772 (10)°	0.18 × 0.13 × 0.09 mm
V = 1367.3 (2) Å3

STOE IPDS-1 diffractometer	5736 independent reflections
Radiation source: fine-focus sealed tube	4365 reflections with I > 2σ(I)
graphite	Rint = 0.040
Phi scans	θmax = 27.0°, θmin = 2.5°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −13→13
Tmin = 0.746, Tmax = 0.841	k = −15→15
12730 measured reflections	l = −16→16

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)] = 0.042	H-atom parameters constrained
wR(F2) = 0.113	w = 1/[σ2(Fo2) + (0.0508P)2 + 3.6107P] where P = (Fo2 + 2Fc2)/3
S = 1.07	(Δ/σ)max = 0.001
5736 reflections	Δρmax = 1.07 e Å−3
301 parameters	Δρmin = −0.87 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0113 (8)

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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	0.58718 (4)	0.60656 (4)	0.33218 (3)	0.02703 (13)
Cd2	0.13789 (4)	0.35828 (4)	0.45817 (4)	0.03022 (14)
N1	0.7929 (5)	0.6709 (5)	0.2127 (5)	0.0374 (12)
C1	0.8391 (7)	0.7302 (7)	0.1166 (7)	0.0464 (16)
S1	0.9043 (3)	0.8167 (3)	−0.0225 (2)	0.0857 (8)
N2	0.3704 (6)	0.2779 (6)	0.4148 (6)	0.0497 (15)
C2	0.4515 (6)	0.2311 (5)	0.3503 (6)	0.0344 (13)
S2	0.5669 (2)	0.1683 (2)	0.2620 (2)	0.0638 (6)
S3	0.23030 (13)	0.59733 (11)	0.45203 (11)	0.0225 (3)
O1	0.3696 (4)	0.5152 (3)	0.4693 (3)	0.0237 (7)
O2	0.1952 (4)	0.6886 (4)	0.5048 (4)	0.0341 (9)
O3	0.1277 (4)	0.5182 (3)	0.5148 (3)	0.0248 (7)
O4	0.2301 (4)	0.6606 (4)	0.3235 (3)	0.0358 (9)
N11	0.4780 (5)	0.7650 (4)	0.3937 (4)	0.0314 (10)
H11A	0.3903	0.7550	0.4365	0.038*
H11B	0.5233	0.7579	0.4461	0.038*
N12	0.4885 (5)	0.7225 (5)	0.1623 (4)	0.0335 (11)
H12	0.3988	0.7116	0.1897	0.040*
N13	0.6435 (5)	0.4318 (5)	0.2982 (4)	0.0328 (11)
H13A	0.7145	0.3756	0.3353	0.039*
H13B	0.5688	0.3957	0.3348	0.039*
C11	0.4672 (7)	0.8939 (6)	0.2973 (6)	0.0451 (16)
H11C	0.5611	0.9083	0.2545	0.054*
H11D	0.4176	0.9555	0.3346	0.054*
C12	0.3922 (7)	0.9159 (6)	0.2065 (6)	0.0490 (17)
H12A	0.3086	0.8818	0.2515	0.059*
H12B	0.3612	1.0079	0.1620	0.059*
C13	0.4749 (7)	0.8584 (6)	0.1151 (6)	0.0457 (16)
H13C	0.4304	0.9011	0.0455	0.055*
H13D	0.5684	0.8747	0.0847	0.055*
C14	0.5532 (7)	0.6788 (7)	0.0627 (5)	0.0433 (15)
H14A	0.6449	0.6991	0.0227	0.052*
H14B	0.4957	0.7254	0.0019	0.052*
C15	0.5708 (8)	0.5377 (7)	0.1047 (6)	0.0468 (17)
H15A	0.4827	0.5156	0.1590	0.056*
H15B	0.5865	0.5210	0.0330	0.056*
C16	0.6857 (8)	0.4500 (7)	0.1701 (6)	0.0454 (16)
H16A	0.7104	0.3676	0.1652	0.054*
H16B	0.7684	0.4857	0.1300	0.054*
N21	0.1109 (6)	0.4989 (5)	0.2712 (4)	0.0381 (12)
H21A	0.0189	0.5387	0.2760	0.046*
H21B	0.1585	0.5590	0.2463	0.046*
N22	0.0976 (5)	0.2022 (5)	0.4261 (5)	0.0375 (12)
H22	0.0022	0.2148	0.4444	0.045*
N23	0.0807 (5)	0.2394 (4)	0.6569 (4)	0.0324 (10)
H23A	0.1097	0.2661	0.6978	0.039*
H23B	−0.0140	0.2544	0.6804	0.039*
C21	0.1564 (8)	0.4493 (7)	0.1779 (6)	0.0502 (17)
H21C	0.2576	0.4155	0.1647	0.060*
H21D	0.1359	0.5191	0.1010	0.060*
C22	0.0864 (9)	0.3446 (8)	0.2112 (6)	0.057 (2)
H22A	−0.0130	0.3704	0.2459	0.068*
H22B	0.0938	0.3378	0.1358	0.068*
C23	0.1440 (7)	0.2160 (7)	0.2992 (7)	0.0475 (17)
H23C	0.1164	0.1521	0.2926	0.057*
H23D	0.2461	0.1990	0.2762	0.057*
C24	0.1475 (7)	0.0726 (6)	0.5072 (7)	0.0476 (17)
H24A	0.2490	0.0549	0.4933	0.057*
H24B	0.1265	0.0146	0.4869	0.057*
C25	0.0848 (8)	0.0459 (6)	0.6396 (7)	0.0489 (17)
H25A	0.1021	−0.0465	0.6857	0.059*
H25B	−0.0164	0.0789	0.6499	0.059*
C26	0.1370 (8)	0.1009 (6)	0.6962 (7)	0.0488 (17)
H26A	0.1094	0.0595	0.7855	0.059*
H26B	0.2391	0.0829	0.6728	0.059*
O31	0.1929 (15)	0.7375 (11)	0.0583 (11)	0.076 (4)	0.50
H31	0.2769	0.7008	0.0475	0.114*	0.50
C31	0.1801 (14)	0.8574 (13)	0.0413 (12)	0.050 (4)	0.50
H31A	0.1703	0.8593	0.1188	0.075*	0.50
H31B	0.0983	0.9125	0.0087	0.075*	0.50
H31C	0.2624	0.8868	−0.0158	0.075*	0.50

	U11	U22	U33	U12	U13	U23
Cd1	0.0291 (2)	0.0297 (2)	0.0207 (2)	−0.00729 (16)	−0.00580 (15)	−0.00850 (15)
Cd2	0.0294 (3)	0.0346 (2)	0.0326 (2)	−0.00777 (17)	−0.00505 (17)	−0.01921 (18)
N1	0.031 (3)	0.052 (3)	0.033 (3)	−0.020 (2)	−0.010 (2)	−0.010 (2)
C1	0.044 (4)	0.062 (4)	0.051 (4)	−0.018 (3)	−0.005 (3)	−0.036 (4)
S1	0.119 (2)	0.107 (2)	0.0407 (11)	−0.0754 (18)	0.0075 (12)	−0.0195 (12)
N2	0.029 (3)	0.070 (4)	0.072 (4)	−0.004 (3)	−0.010 (3)	−0.052 (4)
C2	0.030 (3)	0.033 (3)	0.047 (3)	−0.009 (2)	−0.013 (3)	−0.016 (3)
S2	0.0483 (11)	0.0642 (12)	0.0892 (15)	−0.0107 (9)	0.0066 (10)	−0.0557 (12)
S3	0.0163 (6)	0.0281 (6)	0.0226 (6)	−0.0081 (5)	−0.0038 (4)	−0.0080 (5)
O1	0.0176 (19)	0.0311 (18)	0.0237 (17)	−0.0043 (15)	−0.0064 (14)	−0.0117 (15)
O2	0.023 (2)	0.035 (2)	0.051 (2)	−0.0062 (17)	−0.0077 (17)	−0.0233 (19)
O3	0.0214 (19)	0.0316 (19)	0.0236 (18)	−0.0142 (15)	0.0006 (14)	−0.0111 (15)
O4	0.022 (2)	0.050 (2)	0.0214 (18)	−0.0120 (18)	−0.0080 (15)	0.0009 (17)
N11	0.036 (3)	0.031 (2)	0.033 (2)	−0.012 (2)	−0.007 (2)	−0.015 (2)
N12	0.030 (3)	0.044 (3)	0.018 (2)	−0.017 (2)	−0.0042 (18)	−0.0005 (19)
N13	0.034 (3)	0.040 (3)	0.031 (2)	−0.015 (2)	−0.002 (2)	−0.018 (2)
C11	0.046 (4)	0.027 (3)	0.055 (4)	−0.014 (3)	−0.006 (3)	−0.011 (3)
C12	0.037 (4)	0.034 (3)	0.048 (4)	−0.004 (3)	−0.008 (3)	0.001 (3)
C13	0.044 (4)	0.042 (3)	0.033 (3)	−0.017 (3)	−0.010 (3)	0.004 (3)
C14	0.041 (4)	0.068 (4)	0.020 (3)	−0.027 (3)	−0.002 (2)	−0.010 (3)
C15	0.050 (4)	0.076 (5)	0.030 (3)	−0.031 (4)	−0.002 (3)	−0.026 (3)
C16	0.053 (4)	0.059 (4)	0.035 (3)	−0.025 (3)	0.003 (3)	−0.028 (3)
N21	0.038 (3)	0.046 (3)	0.030 (3)	−0.011 (2)	−0.002 (2)	−0.018 (2)
N22	0.026 (3)	0.045 (3)	0.057 (3)	−0.005 (2)	−0.007 (2)	−0.036 (3)
N23	0.029 (3)	0.035 (3)	0.034 (3)	−0.007 (2)	−0.009 (2)	−0.013 (2)
C21	0.044 (4)	0.070 (5)	0.029 (3)	−0.009 (3)	0.004 (3)	−0.026 (3)
C22	0.059 (5)	0.089 (6)	0.042 (4)	−0.018 (4)	−0.010 (3)	−0.041 (4)
C23	0.038 (4)	0.063 (4)	0.064 (4)	−0.005 (3)	−0.011 (3)	−0.048 (4)
C24	0.043 (4)	0.038 (3)	0.076 (5)	−0.008 (3)	−0.015 (3)	−0.033 (3)
C25	0.047 (4)	0.030 (3)	0.070 (5)	−0.005 (3)	−0.017 (3)	−0.020 (3)
C26	0.055 (5)	0.033 (3)	0.052 (4)	−0.003 (3)	−0.025 (3)	−0.008 (3)
O31	0.101 (11)	0.064 (7)	0.055 (7)	−0.020 (7)	−0.039 (7)	−0.001 (6)
C31	0.034 (8)	0.058 (9)	0.039 (7)	−0.020 (6)	−0.027 (6)	0.014 (6)

Cd1—N11	2.248 (4)	C14—C15	1.528 (10)
Cd1—N13	2.250 (5)	C14—H14A	0.9900
Cd1—N1	2.347 (5)	C14—H14B	0.9900
Cd1—N12	2.351 (5)	C15—C16	1.515 (11)
Cd1—O1i	2.388 (3)	C15—H15A	0.9900
Cd1—O1	2.619 (3)	C15—H15B	0.9900
Cd2—N23	2.247 (5)	C16—H16A	0.9900
Cd2—N21	2.250 (5)	C16—H16B	0.9900
Cd2—N2	2.283 (6)	N21—C21	1.466 (8)
Cd2—N22	2.374 (4)	N21—H21A	0.9200
Cd2—O3	2.386 (3)	N21—H21B	0.9200
Cd2—O3ii	2.676 (4)	N22—C24	1.463 (9)
N1—C1	1.130 (8)	N22—C23	1.475 (8)
C1—S1	1.633 (8)	N22—H22	0.9300
N2—C2	1.169 (8)	N23—C26	1.489 (8)
C2—S2	1.607 (6)	N23—H23A	0.9200
S3—O4	1.458 (4)	N23—H23B	0.9200
S3—O2	1.465 (4)	C21—C22	1.542 (11)
S3—O3	1.485 (3)	C21—H21C	0.9900
S3—O1	1.490 (4)	C21—H21D	0.9900
O1—Cd1i	2.388 (3)	C22—C23	1.508 (11)
N11—C11	1.480 (7)	C22—H22A	0.9900
N11—H11A	0.9200	C22—H22B	0.9900
N11—H11B	0.9200	C23—H23C	0.9900
N12—C13	1.466 (8)	C23—H23D	0.9900
N12—C14	1.480 (8)	C24—C25	1.510 (10)
N12—H12	0.9300	C24—H24A	0.9900
N13—C16	1.476 (7)	C24—H24B	0.9900
N13—H13A	0.9200	C25—C26	1.537 (10)
N13—H13B	0.9200	C25—H25A	0.9900
C11—C12	1.515 (10)	C25—H25B	0.9900
C11—H11C	0.9900	C26—H26A	0.9900
C11—H11D	0.9900	C26—H26B	0.9900
C12—C13	1.515 (10)	O31—C31	1.362 (18)
C12—H12A	0.9900	O31—H31	0.8400
C12—H12B	0.9900	C31—H31A	0.9800
C13—H13C	0.9900	C31—H31B	0.9800
C13—H13D	0.9900	C31—H31C	0.9800
N11—Cd1—N13	164.76 (17)	C15—C14—H14A	108.9
N11—Cd1—N1	99.40 (18)	N12—C14—H14B	108.9
N13—Cd1—N1	95.82 (18)	C15—C14—H14B	108.9
N11—Cd1—N12	89.43 (18)	H14A—C14—H14B	107.7
N13—Cd1—N12	89.82 (18)	C16—C15—C14	117.0 (5)
N1—Cd1—N12	89.72 (17)	C16—C15—H15A	108.0
N11—Cd1—O1i	85.80 (15)	C14—C15—H15A	108.0
N13—Cd1—O1i	91.31 (15)	C16—C15—H15B	108.0
N1—Cd1—O1i	104.15 (15)	C14—C15—H15B	108.0
N12—Cd1—O1i	165.89 (14)	H15A—C15—H15B	107.3
N11—Cd1—O1	84.77 (14)	N13—C16—C15	111.0 (5)
N13—Cd1—O1	80.07 (14)	N13—C16—H16A	109.4
N1—Cd1—O1	175.20 (16)	C15—C16—H16A	109.4
N12—Cd1—O1	92.73 (14)	N13—C16—H16B	109.4
O1i—Cd1—O1	73.63 (13)	C15—C16—H16B	109.4
N23—Cd2—N21	159.07 (19)	H16A—C16—H16B	108.0
N23—Cd2—N2	101.4 (2)	C21—N21—Cd2	116.5 (4)
N21—Cd2—N2	99.3 (2)	C21—N21—H21A	108.2
N23—Cd2—N22	86.47 (18)	Cd2—N21—H21A	108.2
N21—Cd2—N22	90.32 (19)	C21—N21—H21B	108.2
N2—Cd2—N22	90.40 (18)	Cd2—N21—H21B	108.2
N23—Cd2—O3	86.86 (14)	H21A—N21—H21B	107.3
N21—Cd2—O3	92.16 (15)	C24—N22—C23	110.7 (5)
N2—Cd2—O3	101.23 (16)	C24—N22—Cd2	114.7 (4)
N22—Cd2—O3	167.55 (15)	C23—N22—Cd2	114.1 (4)
C1—N1—Cd1	140.6 (5)	C24—N22—H22	105.4
N1—C1—S1	179.4 (9)	C23—N22—H22	105.4
C2—N2—Cd2	138.6 (5)	Cd2—N22—H22	105.4
N2—C2—S2	178.1 (6)	C26—N23—Cd2	116.8 (4)
O4—S3—O2	111.1 (3)	C26—N23—H23A	108.1
O4—S3—O3	108.7 (2)	Cd2—N23—H23A	108.1
O2—S3—O3	109.5 (2)	C26—N23—H23B	108.1
O4—S3—O1	109.9 (2)	Cd2—N23—H23B	108.1
O2—S3—O1	108.6 (2)	H23A—N23—H23B	107.3
O3—S3—O1	109.1 (2)	N21—C21—C22	113.1 (5)
S3—O1—Cd1i	120.41 (19)	N21—C21—H21C	109.0
S3—O1—Cd1	118.74 (19)	C22—C21—H21C	109.0
Cd1i—O1—Cd1	106.37 (13)	N21—C21—H21D	109.0
S3—O3—Cd2	122.13 (19)	C22—C21—H21D	109.0
C11—N11—Cd1	116.2 (4)	H21C—C21—H21D	107.8
C11—N11—H11A	108.2	C23—C22—C21	115.7 (6)
Cd1—N11—H11A	108.2	C23—C22—H22A	108.4
C11—N11—H11B	108.2	C21—C22—H22A	108.4
Cd1—N11—H11B	108.2	C23—C22—H22B	108.4
H11A—N11—H11B	107.4	C21—C22—H22B	108.4
C13—N12—C14	110.3 (5)	H22A—C22—H22B	107.4
C13—N12—Cd1	113.1 (4)	N22—C23—C22	113.7 (5)
C14—N12—Cd1	115.7 (4)	N22—C23—H23C	108.8
C13—N12—H12	105.6	C22—C23—H23C	108.8
C14—N12—H12	105.6	N22—C23—H23D	108.8
Cd1—N12—H12	105.6	C22—C23—H23D	108.8
C16—N13—Cd1	115.9 (4)	H23C—C23—H23D	107.7
C16—N13—H13A	108.3	N22—C24—C25	113.7 (5)
Cd1—N13—H13A	108.3	N22—C24—H24A	108.8
C16—N13—H13B	108.3	C25—C24—H24A	108.8
Cd1—N13—H13B	108.3	N22—C24—H24B	108.8
H13A—N13—H13B	107.4	C25—C24—H24B	108.8
N11—C11—C12	112.4 (5)	H24A—C24—H24B	107.7
N11—C11—H11C	109.1	C24—C25—C26	116.3 (6)
C12—C11—H11C	109.1	C24—C25—H25A	108.2
N11—C11—H11D	109.1	C26—C25—H25A	108.2
C12—C11—H11D	109.1	C24—C25—H25B	108.2
H11C—C11—H11D	107.8	C26—C25—H25B	108.2
C13—C12—C11	115.7 (6)	H25A—C25—H25B	107.4
C13—C12—H12A	108.4	N23—C26—C25	111.9 (6)
C11—C12—H12A	108.4	N23—C26—H26A	109.2
C13—C12—H12B	108.4	C25—C26—H26A	109.2
C11—C12—H12B	108.4	N23—C26—H26B	109.2
H12A—C12—H12B	107.4	C25—C26—H26B	109.2
N12—C13—C12	114.5 (5)	H26A—C26—H26B	107.9
N12—C13—H13C	108.6	C31—O31—H31	109.5
C12—C13—H13C	108.6	O31—C31—H31A	109.5
N12—C13—H13D	108.6	O31—C31—H31B	109.5
C12—C13—H13D	108.6	H31A—C31—H31B	109.5
H13C—C13—H13D	107.6	O31—C31—H31C	109.5
N12—C14—C15	113.4 (5)	H31A—C31—H31C	109.5
N12—C14—H14A	108.9	H31B—C31—H31C	109.5

Table 1

Selected bond lengths (Å)

Cd1—N11	2.248 (4)
Cd1—N13	2.250 (5)
Cd1—N1	2.347 (5)
Cd1—N12	2.351 (5)
Cd1—O1i	2.388 (3)
Cd1—O1	2.619 (3)
Cd2—N23	2.247 (5)
Cd2—N21	2.250 (5)
Cd2—N2	2.283 (6)
Cd2—N22	2.374 (4)
Cd2—O3	2.386 (3)
Cd2—O3ii	2.676 (4)

Symmetry codes: (i) ; (ii) .