catena-Poly[ammonium (cadmium-tri-μ-thio-cyanato-κS:N;κN:S)-1,4,10,13,16-hexa-oxa-cyclo-octa-decane (1/1)].

In the title compound, {(NH(4))[Cd(NCS)(3)]·C(12)H(24)O(6)}(n), the Cd(2+) ion, the ammonium cation, one of the SCN(-) ligands and the macrocycle are located on mirror planes. The thiocyanate anions act as bridging ligands between the Cd(II) ions, leading to a polymeric chain arrangement extending along [001] around a twofold screw axis. The ammonium ions are contained within the bowl of the macrocycle via extensive N-H⋯O hydrogen bonding.

Related literature

For a singly bridged cadmium thio­cyanate complex, see: Bose et al. (2004 ▶). For a triply bridged cadmium thio­cyanate complex, see: Chen et al. (2002 ▶). For an S-bound terminal thio­cyanate cadmium complex, see: Nfor et al. (2006 ▶). For polymeric structures of complexes, see: Lobana et al. (2008 ▶). For the structures and properties of cadmium compounds, see: Gu et al. (2011 ▶); Zheng et al. (2004 ▶); Rajesh et al. (2004 ▶). For bond lengths and angles of related compounds, see: Nawaz et al. (2010 ▶).

Experimental

Crystal data

(NH4)[Cd(NCS)3]·C12H24O6

M = 568.99

Orthorhombic,

a = 14.7568 (6) Å

b = 15.4378 (6) Å

c = 10.6383 (5) Å

V = 2423.54 (18) Å3

Z = 4

Mo Kα radiation

μ = 1.20 mm−1

T = 293 K

0.30 × 0.25 × 0.20 mm

Data collection

Bruker Kappa APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T min = 0.716, T max = 0.796

11323 measured reflections

2483 independent reflections

2445 reflections with I > 2σ(I)

R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.013

wR(F 2) = 0.034

S = 1.09

2483 reflections

154 parameters

5 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.20 e Å−3

Δρmin = −0.36 e Å−3

Absolute structure: Flack (1983 ▶), 7607 Friedel pairs

Flack parameter: 0.005 (15)

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: APEX2 and SAINT (Bruker, 2004 ▶); data reduction: SAINT and XPREP (Bruker, 2004 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and Mercury (Macrae et al., 2006 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶), PLATON (Spek, 2009 ▶) and publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812004898/zb2021sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812004898/zb2021Isup2.hkl

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

(NH4)[Cd(NCS)3]·C12H24O6	F(000) = 1160
Mr = 568.99	Dx = 1.559 Mg m−3
Orthorhombic, Cmc21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 5280 reflections
a = 14.7568 (6) Å	θ = 2.6–26.7°
b = 15.4378 (6) Å	µ = 1.20 mm−1
c = 10.6383 (5) Å	T = 293 K
V = 2423.54 (18) Å3	Block, colourless
Z = 4	0.30 × 0.25 × 0.20 mm

Bruker Kappa APEXII CCD diffractometer	2483 independent reflections
Radiation source: fine-focus sealed tube	2445 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.019
ω and φ scan	θmax = 26.0°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −18→18
Tmin = 0.716, Tmax = 0.796	k = −19→19
11323 measured reflections	l = −13→13

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.013	w = 1/[σ2(Fo2) + (0.020P)2 + 0.1189P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.034	(Δ/σ)max = 0.003
S = 1.09	Δρmax = 0.20 e Å−3
2483 reflections	Δρmin = −0.36 e Å−3
154 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
5 restraints	Extinction coefficient: 0.0058 (2)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), 7607 Friedel pairs
Secondary atom site location: difference Fourier map	Flack parameter: 0.005 (15)

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
C1	0.61632 (10)	1.06679 (10)	0.72484 (14)	0.0337 (3)
C2	0.5000	0.87710 (13)	0.7689 (2)	0.0339 (4)
C3	0.9203 (2)	0.92459 (19)	1.0905 (3)	0.0905 (9)
H3A	0.9205	0.9648	1.1606	0.109*
H3B	0.9177	0.8662	1.1240	0.109*
C4	0.83962 (17)	0.94095 (17)	1.0097 (4)	0.0885 (10)
H4A	0.7851	0.9382	1.0604	0.106*
H4B	0.8436	0.9985	0.9736	0.106*
C5	0.76317 (15)	0.89705 (16)	0.8297 (3)	0.0811 (8)
H5A	0.7709	0.9545	0.7945	0.097*
H5B	0.7062	0.8959	0.8751	0.097*
C6	0.76078 (16)	0.83248 (19)	0.7272 (3)	0.0845 (9)
H6A	0.7596	0.7745	0.7621	0.101*
H6B	0.7065	0.8405	0.6770	0.101*
C7	0.8399 (2)	0.78484 (18)	0.5498 (3)	0.0923 (10)
H7A	0.7847	0.7908	0.5010	0.111*
H7B	0.8430	0.7259	0.5811	0.111*
C8	0.9199 (2)	0.80317 (17)	0.4690 (2)	0.0921 (10)
H8A	0.9185	0.7664	0.3952	0.110*
H8B	0.9186	0.8631	0.4415	0.110*
N1	0.60575 (11)	1.03455 (9)	0.62874 (16)	0.0496 (4)
N2	0.5000	0.91401 (12)	0.86273 (19)	0.0454 (5)
O1	1.0000	0.93509 (16)	1.0190 (3)	0.0776 (8)
O2	0.83461 (10)	0.87912 (10)	0.91271 (18)	0.0692 (4)
O3	0.83851 (11)	0.84297 (10)	0.65100 (18)	0.0703 (4)
O4	1.0000	0.78737 (15)	0.5382 (2)	0.0742 (7)
N3	1.0000	0.80499 (15)	0.8089 (2)	0.0476 (5)
Cd1	0.5000	0.971763 (8)	0.494929 (17)	0.03587 (6)
S1	0.63319 (3)	1.11267 (3)	0.86256 (4)	0.04216 (10)
S2	0.5000	0.82400 (4)	0.63561 (5)	0.04418 (14)
H3E	0.9497 (12)	0.8303 (18)	0.836 (3)	0.096 (10)*
H3C	1.0000	0.7522 (12)	0.844 (3)	0.076 (11)*
H3D	1.0000	0.817 (4)	0.7264 (16)	0.13 (2)*

	U11	U22	U33	U12	U13	U23
C1	0.0298 (7)	0.0389 (8)	0.0324 (7)	−0.0048 (6)	0.0026 (5)	0.0036 (6)
C2	0.0389 (11)	0.0289 (9)	0.0339 (12)	0.000	0.000	0.0067 (9)
C3	0.094 (2)	0.0801 (18)	0.097 (2)	0.0021 (14)	0.0308 (17)	−0.0239 (16)
C4	0.0702 (14)	0.0716 (13)	0.124 (3)	0.0100 (11)	0.035 (2)	−0.025 (2)
C5	0.0397 (11)	0.0731 (14)	0.130 (3)	0.0164 (10)	0.0147 (13)	0.0227 (16)
C6	0.0411 (11)	0.0820 (16)	0.130 (3)	−0.0007 (11)	−0.0205 (13)	0.0190 (17)
C7	0.097 (2)	0.0739 (16)	0.106 (2)	0.0214 (15)	−0.0549 (19)	−0.0204 (15)
C8	0.149 (3)	0.0678 (14)	0.0592 (19)	0.0343 (17)	−0.0297 (17)	−0.0138 (11)
N1	0.0539 (9)	0.0612 (9)	0.0337 (8)	−0.0148 (6)	0.0025 (7)	−0.0026 (7)
N2	0.0682 (13)	0.0370 (9)	0.0309 (9)	0.000	0.000	0.0015 (9)
O1	0.0683 (13)	0.0780 (14)	0.086 (2)	0.000	0.000	−0.0160 (14)
O2	0.0498 (8)	0.0570 (8)	0.1009 (13)	0.0127 (6)	0.0144 (8)	0.0011 (8)
O3	0.0628 (9)	0.0609 (8)	0.0872 (12)	0.0032 (7)	−0.0184 (8)	0.0017 (8)
O4	0.0963 (18)	0.0630 (13)	0.0632 (14)	0.000	0.000	−0.0012 (10)
N3	0.0385 (12)	0.0456 (12)	0.0587 (15)	0.000	0.000	0.0006 (10)
Cd1	0.04531 (9)	0.03708 (8)	0.02522 (8)	0.000	0.000	−0.00054 (7)
S1	0.0465 (2)	0.0454 (2)	0.0346 (2)	−0.00946 (16)	0.00023 (17)	−0.00481 (17)
S2	0.0649 (4)	0.0355 (3)	0.0322 (3)	0.000	0.000	−0.0024 (2)

C1—N1	1.148 (2)	C7—C8	1.488 (4)
C1—S1	1.6463 (15)	C7—H7A	0.9700
C2—N2	1.149 (3)	C7—H7B	0.9700
C2—S2	1.638 (2)	C8—O4	1.413 (3)
C3—O1	1.410 (3)	C8—H8A	0.9700
C3—C4	1.490 (5)	C8—H8B	0.9700
C3—H3A	0.9700	N1—Cd1	2.3241 (16)
C3—H3B	0.9700	N2—Cd1i	2.256 (2)
C4—O2	1.408 (4)	O1—C3ii	1.410 (3)
C4—H4A	0.9700	O4—C8ii	1.413 (3)
C4—H4B	0.9700	N3—H3E	0.888 (10)
C5—O2	1.403 (3)	N3—H3C	0.897 (10)
C5—C6	1.478 (4)	N3—H3D	0.898 (10)
C5—H5A	0.9700	Cd1—N2iii	2.256 (2)
C5—H5B	0.9700	Cd1—N1iv	2.3241 (16)
C6—O3	1.414 (3)	Cd1—S2	2.7283 (6)
C6—H6A	0.9700	Cd1—S1iii	2.7468 (4)
C6—H6B	0.9700	Cd1—S1v	2.7468 (4)
C7—O3	1.402 (3)	S1—Cd1i	2.7468 (4)
N1—C1—S1	179.10 (16)	O4—C8—C7	109.28 (19)
N2—C2—S2	179.69 (19)	O4—C8—H8A	109.8
O1—C3—C4	109.6 (3)	C7—C8—H8A	109.8
O1—C3—H3A	109.7	O4—C8—H8B	109.8
C4—C3—H3A	109.7	C7—C8—H8B	109.8
O1—C3—H3B	109.7	H8A—C8—H8B	108.3
C4—C3—H3B	109.7	C1—N1—Cd1	144.86 (14)
H3A—C3—H3B	108.2	C2—N2—Cd1i	158.30 (17)
O2—C4—C3	110.48 (19)	C3ii—O1—C3	113.1 (4)
O2—C4—H4A	109.6	C5—O2—C4	111.54 (19)
C3—C4—H4A	109.6	C7—O3—C6	112.2 (2)
O2—C4—H4B	109.6	C8—O4—C8ii	113.4 (3)
C3—C4—H4B	109.6	H3E—N3—H3C	105 (2)
H4A—C4—H4B	108.1	H3E—N3—H3D	103 (3)
O2—C5—C6	110.46 (18)	H3C—N3—H3D	127 (5)
O2—C5—H5A	109.6	N2iii—Cd1—N1	93.20 (5)
C6—C5—H5A	109.6	N2iii—Cd1—N1iv	93.20 (5)
O2—C5—H5B	109.6	N1—Cd1—N1iv	84.36 (8)
C6—C5—H5B	109.6	N2iii—Cd1—S2	174.69 (5)
H5A—C5—H5B	108.1	N1—Cd1—S2	90.73 (4)
O3—C6—C5	109.0 (2)	N1iv—Cd1—S2	90.73 (4)
O3—C6—H6A	109.9	N2iii—Cd1—S1iii	92.94 (4)
C5—C6—H6A	109.9	N1—Cd1—S1iii	172.93 (4)
O3—C6—H6B	109.9	N1iv—Cd1—S1iii	91.80 (4)
C5—C6—H6B	109.9	S2—Cd1—S1iii	83.363 (12)
H6A—C6—H6B	108.3	N2iii—Cd1—S1v	92.94 (4)
O3—C7—C8	109.5 (2)	N1—Cd1—S1v	91.80 (4)
O3—C7—H7A	109.8	N1iv—Cd1—S1v	172.93 (4)
C8—C7—H7A	109.8	S2—Cd1—S1v	83.363 (12)
O3—C7—H7B	109.8	S1iii—Cd1—S1v	91.373 (19)
C8—C7—H7B	109.8	C1—S1—Cd1i	98.27 (5)
H7A—C7—H7B	108.2	C2—S2—Cd1	93.24 (7)
O1—C3—C4—O2	63.7 (3)	C1—N1—Cd1—N2iii	107.3 (2)
O2—C5—C6—O3	−67.4 (2)	C1—N1—Cd1—N1iv	14.4 (2)
O3—C7—C8—O4	64.2 (3)	C1—N1—Cd1—S2	−76.3 (2)
C4—C3—O1—C3ii	177.23 (15)	C1—N1—Cd1—S1v	−159.7 (2)
C6—C5—O2—C4	178.6 (2)	N1—Cd1—S2—C2	42.19 (4)
C3—C4—O2—C5	−175.5 (2)	N1iv—Cd1—S2—C2	−42.19 (4)
C8—C7—O3—C6	176.27 (19)	S1iii—Cd1—S2—C2	−133.916 (9)
C5—C6—O3—C7	−178.75 (19)	S1v—Cd1—S2—C2	133.916 (9)
C7—C8—O4—C8ii	−179.93 (16)

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3E···O2	0.89 (1)	2.03 (1)	2.9130 (19)	174 (3)
N3—H3D···O4	0.90 (1)	2.05 (3)	2.892 (3)	155 (5)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N3—H3E⋯O2	0.89 (1)	2.03 (1)	2.9130 (19)	174 (3)
N3—H3D⋯O4	0.90 (1)	2.05 (3)	2.892 (3)	155 (5)