Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229619010945/jx3043sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229619010945/jx3043Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229619010945/jx3043sup3.pdf |
CCDC reference: 1828049
Data collection: APEX3 (Bruker, 2014); cell refinement: APEX3 (Bruker, 2014); data reduction: SAINT (Bruker, 2014); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2016 (Sheldrick, 2015b); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL (Bruker, 2000).
[Zn(C3H3N2S3)2] | Dx = 1.817 Mg m−3 |
Mr = 391.96 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I4 | Cell parameters from 3909 reflections |
a = 18.1367 (12) Å | θ = 2.5–25.8° |
c = 8.7103 (9) Å | µ = 2.57 mm−1 |
V = 2865.2 (5) Å3 | T = 296 K |
Z = 8 | Block, colorless |
F(000) = 1568 | 0.20 × 0.16 × 0.16 mm |
Bruker SMART APEX CCD diffractometer | 2550 reflections with I > 2σ(I) |
phi and ω scans | Rint = 0.032 |
Absorption correction: multi-scan (SADABS; Bruker, 2014) | θmax = 27.2°, θmin = 1.6° |
Tmin = 0.624, Tmax = 0.746 | h = −23→23 |
10994 measured reflections | k = −23→22 |
2908 independent reflections | l = −11→10 |
Refinement on F2 | Hydrogen site location: mixed |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.0273P)2 + 1.9481P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.064 | (Δ/σ)max < 0.001 |
S = 1.04 | Δρmax = 0.31 e Å−3 |
2908 reflections | Δρmin = −0.33 e Å−3 |
155 parameters | Absolute structure: Refined as an inversion twin. |
0 restraints | Absolute structure parameter: 0.32 (2) |
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. Refined as a 2-component inversion twin. The data adsorption correction was carried out by multi-scan techniques using SADABS routine of APEX program (Bruker, 2014). The crystal structure was solved by Shelxt (Sheldrick, 2015a) subprogram using dual space algorithm and refined by full-matrix least-squares on F2 using Shelxl (Sheldrick, 2015b) under the SHELXTL (Bruker, 2000) software package. All non-hydrogen atoms were refined anisotropically with displacement parameters during the final cycles. |
x | y | z | Uiso*/Ueq | ||
Zn4 | 0.500000 | 0.500000 | 0.500000 | 0.0280 (3) | |
Zn3 | 0.500000 | 0.500000 | 1.000000 | 0.0317 (3) | |
S4 | 0.52520 (7) | 0.39832 (7) | 0.84020 (14) | 0.0337 (3) | |
S5 | 0.36726 (8) | 0.34550 (9) | 0.80060 (16) | 0.0483 (4) | |
S6 | 0.22995 (10) | 0.35088 (14) | 0.6101 (2) | 0.0818 (7) | |
N4 | 0.4278 (2) | 0.4347 (2) | 0.6163 (4) | 0.0288 (9) | |
N3 | 0.3570 (2) | 0.4251 (2) | 0.5583 (5) | 0.0351 (10) | |
C4 | 0.4419 (3) | 0.3974 (2) | 0.7436 (6) | 0.0308 (10) | |
C5 | 0.3197 (3) | 0.3792 (3) | 0.6432 (6) | 0.0430 (13) | |
C6 | 0.2128 (4) | 0.3882 (4) | 0.4237 (9) | 0.082 (2) | |
H6A | 0.243705 | 0.363986 | 0.349855 | 0.123* | |
H6B | 0.223365 | 0.440066 | 0.424045 | 0.123* | |
H6C | 0.161965 | 0.380636 | 0.396955 | 0.123* | |
Zn2 | 1.000000 | 0.500000 | 0.750000 | 0.0275 (2) | |
Zn1 | 1.000000 | 0.500000 | 1.250000 | 0.0307 (3) | |
S1 | 0.95148 (8) | 0.59642 (7) | 1.10196 (16) | 0.0368 (3) | |
S2 | 0.79737 (8) | 0.53882 (9) | 1.03997 (15) | 0.0451 (4) | |
S3 | 0.70135 (8) | 0.44608 (10) | 0.83252 (18) | 0.0513 (4) | |
N1 | 0.8472 (2) | 0.4695 (2) | 0.8064 (4) | 0.0330 (10) | |
N2 | 0.9062 (2) | 0.5067 (2) | 0.8707 (5) | 0.0311 (9) | |
C1 | 0.8903 (2) | 0.5448 (2) | 0.9943 (6) | 0.0294 (10) | |
C2 | 0.7868 (3) | 0.4817 (3) | 0.8825 (6) | 0.0350 (12) | |
C3 | 0.7250 (3) | 0.4016 (4) | 0.6546 (8) | 0.0606 (18) | |
H3A | 0.742644 | 0.437759 | 0.583021 | 0.091* | |
H3B | 0.682097 | 0.377793 | 0.613151 | 0.091* | |
H3C | 0.762732 | 0.365583 | 0.672783 | 0.091* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn4 | 0.0299 (4) | 0.0299 (4) | 0.0241 (6) | 0.000 | 0.000 | 0.000 |
Zn3 | 0.0351 (4) | 0.0351 (4) | 0.0249 (6) | 0.000 | 0.000 | 0.000 |
S4 | 0.0337 (7) | 0.0364 (7) | 0.0310 (7) | 0.0030 (6) | −0.0034 (6) | −0.0030 (5) |
S5 | 0.0457 (8) | 0.0616 (10) | 0.0377 (8) | −0.0195 (7) | −0.0040 (6) | 0.0160 (7) |
S6 | 0.0449 (10) | 0.1328 (19) | 0.0677 (12) | −0.0372 (11) | −0.0127 (9) | 0.0203 (12) |
N4 | 0.029 (2) | 0.034 (2) | 0.024 (2) | −0.0016 (18) | −0.0017 (17) | −0.0011 (18) |
N3 | 0.033 (2) | 0.044 (3) | 0.028 (2) | 0.0017 (19) | 0.0014 (18) | −0.0020 (19) |
C4 | 0.034 (3) | 0.029 (2) | 0.030 (3) | −0.0013 (19) | 0.006 (2) | −0.005 (2) |
C5 | 0.036 (3) | 0.059 (3) | 0.034 (3) | −0.008 (3) | −0.001 (2) | 0.000 (3) |
C6 | 0.051 (4) | 0.098 (6) | 0.098 (6) | 0.008 (4) | −0.038 (4) | 0.006 (5) |
Zn2 | 0.0271 (3) | 0.0271 (3) | 0.0284 (6) | 0.000 | 0.000 | 0.000 |
Zn1 | 0.0342 (4) | 0.0342 (4) | 0.0237 (6) | 0.000 | 0.000 | 0.000 |
S1 | 0.0430 (8) | 0.0327 (7) | 0.0347 (7) | −0.0031 (6) | −0.0095 (6) | 0.0020 (5) |
S2 | 0.0305 (7) | 0.0719 (10) | 0.0329 (7) | 0.0005 (7) | 0.0046 (6) | −0.0105 (7) |
S3 | 0.0309 (8) | 0.0835 (12) | 0.0396 (8) | −0.0152 (7) | −0.0043 (6) | 0.0014 (8) |
N1 | 0.027 (2) | 0.042 (2) | 0.030 (2) | −0.0039 (18) | −0.0022 (18) | 0.0001 (18) |
N2 | 0.029 (2) | 0.036 (2) | 0.029 (2) | −0.0003 (17) | −0.0004 (18) | −0.0008 (19) |
C1 | 0.028 (2) | 0.033 (3) | 0.027 (2) | 0.0001 (19) | −0.003 (2) | 0.007 (2) |
C2 | 0.031 (3) | 0.045 (3) | 0.029 (3) | −0.003 (2) | −0.006 (2) | 0.004 (2) |
C3 | 0.049 (4) | 0.077 (5) | 0.056 (4) | −0.006 (3) | −0.019 (3) | −0.015 (3) |
Zn4—N4 | 2.036 (4) | Zn2—N2 | 2.004 (4) |
Zn4—N4i | 2.036 (4) | Zn2—N2vi | 2.004 (4) |
Zn4—N4ii | 2.036 (4) | Zn2—N2vii | 2.004 (4) |
Zn4—N4iii | 2.036 (4) | Zn2—N2viii | 2.004 (4) |
Zn3—S4 | 2.3551 (13) | Zn1—S1 | 2.3442 (13) |
Zn3—S4iv | 2.3552 (13) | Zn1—S1ix | 2.3442 (13) |
Zn3—S4v | 2.3552 (13) | Zn1—S1vii | 2.3442 (13) |
Zn3—S4i | 2.3552 (13) | Zn1—S1x | 2.3442 (13) |
S4—C4 | 1.730 (5) | S1—C1 | 1.728 (5) |
S5—C4 | 1.722 (5) | S2—C2 | 1.730 (5) |
S5—C5 | 1.732 (5) | S2—C1 | 1.736 (5) |
S6—C5 | 1.730 (5) | S3—C2 | 1.734 (5) |
S6—C6 | 1.787 (8) | S3—C3 | 1.798 (6) |
N4—C4 | 1.324 (7) | N1—C2 | 1.299 (6) |
N4—N3 | 1.391 (5) | N1—N2 | 1.383 (5) |
N3—C5 | 1.304 (6) | N2—C1 | 1.311 (6) |
C6—H6A | 0.9600 | C3—H3A | 0.9600 |
C6—H6B | 0.9599 | C3—H3B | 0.9600 |
C6—H6C | 0.9600 | C3—H3C | 0.9600 |
N4—Zn4—N4i | 120.3 (2) | N2—Zn2—N2vi | 105.99 (11) |
N4—Zn4—N4ii | 104.35 (10) | N2—Zn2—N2vii | 116.7 (2) |
N4i—Zn4—N4ii | 104.35 (10) | N2vi—Zn2—N2vii | 105.99 (11) |
N4—Zn4—N4iii | 104.35 (10) | N2—Zn2—N2viii | 105.99 (11) |
N4i—Zn4—N4iii | 104.35 (10) | N2vi—Zn2—N2viii | 116.7 (2) |
N4ii—Zn4—N4iii | 120.3 (2) | N2vii—Zn2—N2viii | 105.99 (11) |
S4—Zn3—S4iv | 110.44 (3) | S1—Zn1—S1ix | 107.61 (3) |
S4—Zn3—S4v | 110.44 (3) | S1—Zn1—S1vii | 113.26 (7) |
S4iv—Zn3—S4v | 107.55 (6) | S1ix—Zn1—S1vii | 107.61 (3) |
S4—Zn3—S4i | 107.55 (6) | S1—Zn1—S1x | 107.61 (3) |
S4iv—Zn3—S4i | 110.44 (3) | S1ix—Zn1—S1x | 113.26 (7) |
S4v—Zn3—S4i | 110.44 (3) | S1vii—Zn1—S1x | 107.61 (3) |
C4—S4—Zn3 | 97.21 (16) | C1—S1—Zn1 | 97.79 (16) |
C4—S5—C5 | 88.3 (3) | C2—S2—C1 | 87.9 (2) |
C5—S6—C6 | 101.7 (3) | C2—S3—C3 | 99.8 (3) |
C4—N4—N3 | 114.7 (4) | C2—N1—N2 | 111.3 (4) |
C4—N4—Zn4 | 126.2 (3) | C1—N2—N1 | 114.8 (4) |
N3—N4—Zn4 | 119.1 (3) | C1—N2—Zn2 | 130.5 (3) |
C5—N3—N4 | 110.7 (4) | N1—N2—Zn2 | 114.5 (3) |
N4—C4—S5 | 111.7 (4) | N2—C1—S1 | 126.2 (4) |
N4—C4—S4 | 124.8 (4) | N2—C1—S2 | 111.6 (4) |
S5—C4—S4 | 123.5 (3) | S1—C1—S2 | 122.2 (3) |
N3—C5—S6 | 125.7 (4) | N1—C2—S2 | 114.4 (4) |
N3—C5—S5 | 114.6 (4) | N1—C2—S3 | 124.2 (4) |
S6—C5—S5 | 119.7 (3) | S2—C2—S3 | 121.4 (3) |
S6—C6—H6A | 109.5 | S3—C3—H3A | 109.5 |
S6—C6—H6B | 109.5 | S3—C3—H3B | 109.5 |
H6A—C6—H6B | 109.5 | H3A—C3—H3B | 109.5 |
S6—C6—H6C | 109.5 | S3—C3—H3C | 109.5 |
H6A—C6—H6C | 109.5 | H3A—C3—H3C | 109.5 |
H6B—C6—H6C | 109.5 | H3B—C3—H3C | 109.5 |
C4—N4—N3—C5 | −1.1 (6) | C2—N1—N2—C1 | 1.1 (6) |
Zn4—N4—N3—C5 | 177.0 (3) | C2—N1—N2—Zn2 | −174.1 (3) |
N3—N4—C4—S5 | 0.9 (5) | N1—N2—C1—S1 | 179.5 (3) |
Zn4—N4—C4—S5 | −177.2 (2) | Zn2—N2—C1—S1 | −6.2 (7) |
N3—N4—C4—S4 | 179.6 (3) | N1—N2—C1—S2 | −1.2 (5) |
Zn4—N4—C4—S4 | 1.5 (6) | Zn2—N2—C1—S2 | 173.1 (3) |
C5—S5—C4—N4 | −0.3 (4) | Zn1—S1—C1—N2 | −82.5 (4) |
C5—S5—C4—S4 | −179.0 (4) | Zn1—S1—C1—S2 | 98.2 (3) |
Zn3—S4—C4—N4 | 89.0 (4) | C2—S2—C1—N2 | 0.7 (4) |
Zn3—S4—C4—S5 | −92.5 (3) | C2—S2—C1—S1 | −179.9 (3) |
N4—N3—C5—S6 | −179.0 (4) | N2—N1—C2—S2 | −0.6 (5) |
N4—N3—C5—S5 | 0.9 (6) | N2—N1—C2—S3 | 178.3 (3) |
C6—S6—C5—N3 | 8.9 (6) | C1—S2—C2—N1 | −0.1 (4) |
C6—S6—C5—S5 | −170.9 (4) | C1—S2—C2—S3 | −179.0 (3) |
C4—S5—C5—N3 | −0.4 (4) | C3—S3—C2—N1 | −4.7 (5) |
C4—S5—C5—S6 | 179.5 (4) | C3—S3—C2—S2 | 174.1 (3) |
Symmetry codes: (i) −x+1, −y+1, z; (ii) −y+1, x, −z+1; (iii) y, −x+1, −z+1; (iv) −y+1, x, −z+2; (v) y, −x+1, −z+2; (vi) −y+3/2, x−1/2, −z+3/2; (vii) −x+2, −y+1, z; (viii) y+1/2, −x+3/2, −z+3/2; (ix) y+1/2, −x+3/2, −z+5/2; (x) −y+3/2, x−1/2, −z+5/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3C···S6xi | 0.96 | 3.02 | 3.887 (7) | 151 |
C3—H3B···N3ii | 0.96 | 2.48 | 3.392 (7) | 158 |
C6—H6B···S1xii | 0.96 | 3.04 | 3.599 (7) | 119 |
C6—H6B···S1xii | 0.96 | 3.04 | 3.599 (7) | 119 |
C3—H3B···N3ii | 0.96 | 2.48 | 3.392 (7) | 158 |
C3—H3C···S6xi | 0.96 | 3.02 | 3.887 (7) | 151 |
Symmetry codes: (ii) −y+1, x, −z+1; (xi) y+1/2, −x+1/2, −z+3/2; (xii) y−1/2, −x+3/2, −z+3/2. |