catena-Poly[[[bis-(thio-cyanato-κN)zinc]bis-[μ-1,3,5-tris-(1H-1,2,4-triazol-1-yl-meth-yl)benzene-κ(2)N(4):N(4')]] mono-hydrate].

In the title complex, {[Zn(NCS)(2)(C(15)H(15)N(9))(2)]·H(2)O}(n), the Zn(II) ion is located on an inversion centre and is six-coordinated in a distorted octa-hedral geometry, coordinated by N atoms from four bridging 1,3,5-tris-(1,2,4-triazol-1-ylmeth-yl)benzene (ttmb) ligands and two terminal SCN(-) counter-anions. Two of the three triazol groups in each ttmb ligand link the Zn(II) atoms, forming a looped-chain structure along [0-11]. The lattice water molecule shows half-occupancy due to disorder around an inversion centre.

Related literature

For background to the use of flexible tripodal compounds in the design and construction of compounds with metal-organic framework structures, see: Moon et al. (2006 ▶); Xu et al. (2009 ▶). For similar structures, see: Yin et al. (2009 ▶); Shi et al. (2011 ▶).

Experimental

Crystal data

[Zn(NCS)2(C15H15N9)2]·H2O

M = 842.27

Triclinic,

a = 8.5766 (17) Å

b = 9.5036 (19) Å

c = 11.723 (2) Å

α = 80.01 (3)°

β = 85.40 (3)°

γ = 89.55 (3)°

V = 938.0 (3) Å3

Z = 1

Mo Kα radiation

μ = 0.83 mm−1

T = 293 K

0.20 × 0.18 × 0.16 mm

Data collection

Rigaku Saturn724 diffractometer

Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006 ▶) T min = 0.852, T max = 0.879

11566 measured reflections

4444 independent reflections

3972 reflections with I > 2σ(I)

R int = 0.024

Refinement

R[F 2 > 2σ(F 2)] = 0.041

wR(F 2) = 0.108

S = 1.05

4444 reflections

265 parameters

9 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.61 e Å−3

Δρmin = −0.39 e Å−3

Data collection: CrystalClear (Rigaku/MSC, 2006 ▶); cell refinement: CrystalClear (Rigaku/MSC, 2006 ▶); data reduction: CrystalClear (Rigaku/MSC, 2006 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: CrystalStructure (Rigaku/MSC, 2006 ▶); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2006 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812039256/ds2211sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812039256/ds2211Isup2.hkl

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

[Zn(NCS)2(C15H15N9)2]·H2O	Z = 1
Mr = 842.27	F(000) = 434
Triclinic, P1	Dx = 1.491 Mg m−3
a = 8.5766 (17) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.5036 (19) Å	Cell parameters from 2773 reflections
c = 11.723 (2) Å	θ = 2.2–27.9°
α = 80.01 (3)°	µ = 0.83 mm−1
β = 85.40 (3)°	T = 293 K
γ = 89.55 (3)°	Prism, colorless
V = 938.0 (3) Å3	0.20 × 0.18 × 0.16 mm

Rigaku Saturn724 diffractometer	4444 independent reflections
Radiation source: fine-focus sealed tube	3972 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
Detector resolution: 28.5714 pixels mm-1	θmax = 27.9°, θmin = 2.2°
ω and φ scans	h = −11→11
Absorption correction: multi-scan ?	k = −12→12
Tmin = 0.852, Tmax = 0.879	l = −15→15
11566 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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ2(Fo2) + (0.0517P)2 + 0.3475P] where P = (Fo2 + 2Fc2)/3
4444 reflections	(Δ/σ)max < 0.001
265 parameters	Δρmax = 0.61 e Å−3
9 restraints	Δρmin = −0.39 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	Occ. (<1)
Zn1	0.0000	1.0000	0.0000	0.03753 (14)
N1	−0.1335 (3)	1.0823 (3)	0.1368 (2)	0.0516 (6)
N2	0.1925 (2)	0.9400 (2)	0.11113 (18)	0.0398 (5)
N3	0.3170 (2)	0.8611 (2)	0.26349 (17)	0.0374 (4)
N4	0.4133 (3)	0.8369 (3)	0.1727 (2)	0.0561 (7)
N5	0.2223 (3)	0.2854 (2)	0.3054 (2)	0.0431 (5)
N8	0.0899 (2)	1.2105 (2)	−0.06854 (18)	0.0397 (5)
N9	0.0847 (3)	1.4448 (3)	−0.1391 (2)	0.0579 (7)
N10	0.2207 (3)	1.3860 (2)	−0.17586 (18)	0.0395 (5)
O1	0.5990 (11)	0.4298 (9)	0.9817 (9)	0.135 (3)	0.50
C2	0.1872 (3)	0.9224 (3)	0.2261 (2)	0.0404 (5)
H2	0.1043	0.9494	0.2736	0.049*
C3	0.3328 (3)	0.8857 (4)	0.0833 (2)	0.0527 (7)
H3	0.3701	0.8829	0.0070	0.063*
C4	0.3613 (4)	0.8227 (3)	0.3821 (2)	0.0444 (6)
H4B	0.3159	0.8913	0.4273	0.053*
H4A	0.4742	0.8302	0.3812	0.053*
C5	0.3110 (3)	0.6738 (2)	0.4421 (2)	0.0343 (5)
C6	0.3413 (3)	0.6377 (2)	0.5581 (2)	0.0350 (5)
H6	0.3910	0.7036	0.5933	0.042*
C7	0.2990 (3)	0.5056 (3)	0.6222 (2)	0.0357 (5)
C8	0.2262 (3)	0.4067 (3)	0.5681 (2)	0.0396 (5)
H8	0.1982	0.3171	0.6103	0.048*
C9	0.1954 (3)	0.4408 (3)	0.4526 (2)	0.0385 (5)
C10	0.2379 (3)	0.5756 (3)	0.3897 (2)	0.0381 (5)
H10	0.2168	0.5993	0.3121	0.046*
C11	0.1173 (3)	0.3323 (3)	0.3945 (3)	0.0466 (6)
H11B	0.0839	0.2503	0.4527	0.056*
H11A	0.0251	0.3744	0.3599	0.056*
C14	0.3404 (3)	0.4707 (3)	0.7471 (2)	0.0458 (6)
H14A	0.4382	0.4187	0.7498	0.055*
H14B	0.3564	0.5592	0.7753	0.055*
C15	0.0108 (4)	1.3348 (3)	−0.0744 (3)	0.0528 (7)
H15	−0.0874	1.3420	−0.0360	0.063*
C16	0.2207 (3)	1.2478 (3)	−0.1330 (2)	0.0412 (6)
H16	0.3017	1.1857	−0.1465	0.049*
C1	−0.1657 (3)	1.0544 (3)	0.2354 (2)	0.0422 (6)
N6	0.3491 (3)	0.2042 (3)	0.3333 (2)	0.0560 (6)
N7	0.3519 (4)	0.2694 (3)	0.1395 (3)	0.0728 (8)
C12	0.4207 (4)	0.1989 (4)	0.2304 (3)	0.0599 (8)
H12	0.5134	0.1490	0.2217	0.072*
C13	0.2266 (5)	0.3210 (4)	0.1909 (3)	0.0661 (9)
H13	0.1508	0.3756	0.1514	0.079*
H1A	0.517 (7)	0.391 (8)	1.021 (7)	0.099*	0.50
H1B	0.588 (10)	0.5203 (18)	0.969 (8)	0.099*	0.50
S1	−0.21123 (13)	1.00586 (11)	0.37384 (7)	0.0710 (3)

	U11	U22	U33	U12	U13	U23
Zn1	0.0382 (2)	0.0368 (2)	0.0329 (2)	0.00232 (16)	−0.00183 (16)	0.00624 (15)
N1	0.0540 (14)	0.0583 (15)	0.0387 (12)	0.0090 (11)	0.0033 (11)	−0.0010 (11)
N2	0.0371 (11)	0.0417 (11)	0.0377 (11)	0.0018 (9)	−0.0051 (9)	0.0024 (9)
N3	0.0422 (11)	0.0363 (10)	0.0313 (10)	0.0001 (8)	−0.0048 (8)	0.0018 (8)
N4	0.0436 (13)	0.0825 (19)	0.0403 (12)	0.0183 (12)	−0.0039 (10)	−0.0054 (12)
N5	0.0470 (12)	0.0392 (11)	0.0464 (12)	0.0006 (9)	−0.0147 (10)	−0.0112 (9)
N8	0.0418 (11)	0.0370 (11)	0.0364 (10)	0.0007 (9)	−0.0020 (9)	0.0040 (8)
N9	0.0670 (16)	0.0378 (12)	0.0624 (16)	0.0086 (11)	0.0138 (13)	0.0002 (11)
N10	0.0450 (12)	0.0347 (10)	0.0358 (10)	−0.0016 (9)	−0.0034 (9)	0.0023 (8)
O1	0.147 (7)	0.097 (5)	0.142 (7)	−0.010 (5)	0.029 (6)	0.012 (5)
C2	0.0390 (13)	0.0412 (13)	0.0391 (13)	0.0037 (10)	−0.0015 (10)	−0.0019 (10)
C3	0.0417 (15)	0.079 (2)	0.0343 (13)	0.0104 (14)	−0.0010 (11)	−0.0011 (13)
C4	0.0587 (16)	0.0396 (13)	0.0333 (12)	−0.0075 (12)	−0.0109 (11)	0.0017 (10)
C5	0.0352 (12)	0.0323 (11)	0.0340 (11)	0.0014 (9)	−0.0028 (9)	−0.0019 (9)
C6	0.0365 (12)	0.0337 (11)	0.0345 (12)	−0.0018 (9)	−0.0060 (9)	−0.0034 (9)
C7	0.0360 (12)	0.0356 (12)	0.0336 (11)	−0.0013 (9)	−0.0033 (9)	−0.0004 (9)
C8	0.0412 (13)	0.0328 (12)	0.0425 (13)	−0.0024 (10)	−0.0027 (11)	−0.0003 (10)
C9	0.0358 (12)	0.0368 (12)	0.0439 (13)	−0.0017 (10)	−0.0028 (10)	−0.0098 (10)
C10	0.0435 (13)	0.0380 (12)	0.0330 (12)	0.0014 (10)	−0.0068 (10)	−0.0055 (10)
C11	0.0446 (15)	0.0441 (14)	0.0535 (16)	−0.0052 (11)	−0.0081 (12)	−0.0131 (12)
C14	0.0505 (15)	0.0461 (14)	0.0368 (13)	−0.0133 (12)	−0.0084 (11)	0.0072 (11)
C15	0.0564 (17)	0.0432 (15)	0.0531 (16)	0.0054 (12)	0.0138 (13)	−0.0011 (12)
C16	0.0390 (13)	0.0381 (13)	0.0426 (13)	0.0035 (10)	−0.0054 (11)	0.0050 (10)
C1	0.0423 (14)	0.0388 (13)	0.0457 (14)	0.0095 (10)	−0.0019 (11)	−0.0090 (11)
N6	0.0552 (15)	0.0525 (14)	0.0631 (16)	0.0080 (11)	−0.0175 (13)	−0.0127 (12)
N7	0.089 (2)	0.074 (2)	0.0569 (17)	0.0002 (17)	0.0022 (16)	−0.0172 (15)
C12	0.0532 (18)	0.0542 (18)	0.078 (2)	−0.0016 (14)	−0.0063 (16)	−0.0266 (16)
C13	0.086 (2)	0.063 (2)	0.0518 (18)	0.0154 (18)	−0.0215 (17)	−0.0102 (15)
S1	0.0963 (6)	0.0730 (5)	0.0395 (4)	0.0230 (5)	0.0105 (4)	−0.0065 (4)

Zn1—N8	2.146 (2)	C4—H4B	0.9700
Zn1—N8i	2.146 (2)	C4—H4A	0.9700
Zn1—N1	2.149 (2)	C5—C10	1.383 (3)
Zn1—N1i	2.149 (2)	C5—C6	1.390 (3)
Zn1—N2i	2.196 (2)	C6—C7	1.382 (3)
Zn1—N2	2.196 (2)	C6—H6	0.9300
N1—C1	1.152 (3)	C7—C8	1.398 (3)
N2—C2	1.327 (3)	C7—C14	1.515 (3)
N2—C3	1.344 (3)	C8—C9	1.383 (4)
N3—C2	1.322 (3)	C8—H8	0.9300
N3—N4	1.346 (3)	C9—C10	1.398 (3)
N3—C4	1.455 (3)	C9—C11	1.518 (3)
N4—C3	1.316 (4)	C10—H10	0.9300
N5—C13	1.324 (4)	C11—H11B	0.9700
N5—N6	1.357 (3)	C11—H11A	0.9700
N5—C11	1.452 (4)	C14—N10iii	1.459 (3)
N8—C16	1.316 (3)	C14—H14A	0.9700
N8—C15	1.353 (4)	C14—H14B	0.9700
N9—C15	1.314 (4)	C15—H15	0.9300
N9—N10	1.361 (3)	C16—H16	0.9300
N10—C16	1.322 (3)	C1—S1	1.625 (3)
N10—C14ii	1.459 (3)	N6—C12	1.317 (4)
O1—H1A	0.853 (13)	N7—C13	1.322 (5)
O1—H1B	0.853 (13)	N7—C12	1.334 (5)
C2—H2	0.9300	C12—H12	0.9300
C3—H3	0.9300	C13—H13	0.9300
C4—C5	1.516 (3)
N8—Zn1—N8i	180.0	C10—C5—C6	119.5 (2)
N8—Zn1—N1	89.99 (9)	C10—C5—C4	124.7 (2)
N8i—Zn1—N1	90.01 (9)	C6—C5—C4	115.9 (2)
N8—Zn1—N1i	90.01 (9)	C7—C6—C5	121.1 (2)
N8i—Zn1—N1i	89.99 (9)	C7—C6—H6	119.5
N1—Zn1—N1i	180.0	C5—C6—H6	119.5
N8—Zn1—N2i	85.29 (8)	C6—C7—C8	119.0 (2)
N8i—Zn1—N2i	94.71 (8)	C6—C7—C14	118.5 (2)
N1—Zn1—N2i	88.53 (9)	C8—C7—C14	122.4 (2)
N1i—Zn1—N2i	91.47 (9)	C9—C8—C7	120.6 (2)
N8—Zn1—N2	94.71 (8)	C9—C8—H8	119.7
N8i—Zn1—N2	85.29 (8)	C7—C8—H8	119.7
N1—Zn1—N2	91.47 (9)	C8—C9—C10	119.4 (2)
N1i—Zn1—N2	88.53 (9)	C8—C9—C11	120.2 (2)
N2i—Zn1—N2	180.00 (11)	C10—C9—C11	120.4 (2)
C1—N1—Zn1	140.3 (2)	C5—C10—C9	120.4 (2)
C2—N2—C3	102.6 (2)	C5—C10—H10	119.8
C2—N2—Zn1	127.61 (18)	C9—C10—H10	119.8
C3—N2—Zn1	128.64 (18)	N5—C11—C9	111.5 (2)
C2—N3—N4	109.9 (2)	N5—C11—H11B	109.3
C2—N3—C4	128.9 (2)	C9—C11—H11B	109.3
N4—N3—C4	121.2 (2)	N5—C11—H11A	109.3
C3—N4—N3	102.6 (2)	C9—C11—H11A	109.3
C13—N5—N6	108.7 (3)	H11B—C11—H11A	108.0
C13—N5—C11	129.8 (3)	N10iii—C14—C7	113.3 (2)
N6—N5—C11	121.1 (2)	N10iii—C14—H14A	108.9
C16—N8—C15	103.1 (2)	C7—C14—H14A	108.9
C16—N8—Zn1	128.82 (18)	N10iii—C14—H14B	108.9
C15—N8—Zn1	126.93 (19)	C7—C14—H14B	108.9
C15—N9—N10	102.7 (2)	H14A—C14—H14B	107.7
C16—N10—N9	109.5 (2)	N9—C15—N8	114.2 (3)
C16—N10—C14ii	128.6 (2)	N9—C15—H15	122.9
N9—N10—C14ii	121.8 (2)	N8—C15—H15	122.9
H1A—O1—H1B	109 (3)	N8—C16—N10	110.5 (2)
N2—C2—N3	110.2 (2)	N8—C16—H16	124.8
N2—C2—H2	124.9	N10—C16—H16	124.8
N3—C2—H2	124.9	N1—C1—S1	176.9 (3)
N4—C3—N2	114.6 (2)	C12—N6—N5	102.2 (3)
N4—C3—H3	122.7	C13—N7—C12	101.6 (3)
N2—C3—H3	122.7	N6—C12—N7	115.9 (3)
N3—C4—C5	114.5 (2)	N6—C12—H12	122.1
N3—C4—H4B	108.6	N7—C12—H12	122.1
C5—C4—H4B	108.6	N5—C13—N7	111.6 (3)
N3—C4—H4A	108.6	N5—C13—H13	124.2
C5—C4—H4A	108.6	N7—C13—H13	124.2
H4B—C4—H4A	107.6