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The successful application of the newly developed image-plate neutron Laue diffractometer (LADI) at the Institut Laue-Langevin (ILL), Grenoble, France, for rapid hydrogen-bonding characterization is reported. The case study concerns the promising non-linear optical material zinc (tris)thiourea sulfate (ZTS), which contains 30 atoms in the asymmetric unit and crystallizes in the orthorhombic space group, Pca21, a = 11.0616 (9), b = 7.7264 (6), c = 15.558 (1) Å [T = 100.0 (1) K]. The results from a 12 h data collection from ZTS on LADI are compared with those obtained over 135 h using the monochromatic four-circle diffractometer D9 at the same reactor source with a crystal 13 times larger in volume. Both studies reveal the extensive hydrogen bonding and other close non-bonded contacts within the material. As expected, the results from D9 are more precise than those obtained from LADI; however, the bond geometry determined from the two experiments is the same within the larger estimated standard deviations. Furthermore, the conclusions drawn from the two studies separately regarding the nature of all supramolecular features are identical. This illustrates that LADI is eminently suitable for rapid characterization of hydrogen-bonded structures by neutron diffraction, with the gain in speed compared with traditional instrumentation being several orders of magnitude.
Supporting information
 | Crystallographic Information File (CIF) https://doi.org/10.1107/S010876730100349X/bk0089sup1.cif |
 | Structure factor file (SHELXL table format) https://doi.org/10.1107/S010876730100349X/bk0089ladisup2.sft |
| Structure factor file (SHELXL table format) https://doi.org/10.1107/S010876730100349X/bk0089d9sup3.sft |
 | Portable Document Format (PDF) file https://doi.org/10.1107/S010876730100349X/bk0089sup4.pdf |
Computing details top
Data collection: MAD (Barthelemy, 1984); cell refinement: RAFD9 (local program); data reduction: RACER (Wilkinson et al., 1988); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL-Plus (Sheldrick, 1995); software used to prepare material for publication: SHELXL93 (Sheldrick, 1993).
D9zts(100K) top
Crystal data top
| C3H12N6O4S4Zn | F(000) = 324 |
| Mr = 389.40 | Dx = 1.945 Mg m−3 |
| Orthorhombic, Pca21 | Neutrons radiation, λ = 0.8369 Å |
| a = 11.0616 (9) Å | µ = 0.13 mm−1 |
| b = 7.7264 (6) Å | T = 100 K |
| c = 15.558 (1) Å | Truncated square prism, transparent |
| V = 1329.7 (2) Å3 | 4.1 × 2.8 × 2.1 mm |
| Z = 4 |
Data collection top
| High-flux four-circle diffractometer, D9 | 3217 reflections with I > 2σ(I) |
| Radiation source: D9 at the Institut Laue Langevin reactor, Grenoble, France | Rint = 0.026 |
| Cu(220) crystal monochromator | θmax = 49.2°, θmin = 3.8° |
| ω–x–θ scans | h = −18→20 |
| Absorption correction: analytical: DATAP (coppens, 1970) ? | k = −12→13 |
| Tmin = 0.712, Tmax = 0.785 | l = −5→26 |
| 4454 measured reflections | 1 standard reflections every 50 reflections |
| 3503 independent reflections | intensity decay: none |
Refinement top
| Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
| Least-squares matrix: full | All H-atom parameters refined |
| R[F2 > 2σ(F2)] = 0.035 | Calculated w = 1/[σ2(Fo2) + (0.P)2] where P = (Fo2 + 2Fc2)/3 |
| wR(F2) = 0.069 | (Δ/σ)max = −0.022 |
| S = 1.56 | Δρmax = 0.90 e Å−3 |
| 3493 reflections | Δρmin = −0.90 e Å−3 |
| 272 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 1 restraint | Extinction coefficient: 0.0290 (5) |
| Primary atom site location: none (taken from XRD data) | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
| Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.00 (999) |
Crystal data top
| C3H12N6O4S4Zn | V = 1329.7 (2) Å3 |
| Mr = 389.40 | Z = 4 |
| Orthorhombic, Pca21 | Neutrons radiation, λ = 0.8369 Å |
| a = 11.0616 (9) Å | µ = 0.13 mm−1 |
| b = 7.7264 (6) Å | T = 100 K |
| c = 15.558 (1) Å | 4.1 × 2.8 × 2.1 mm |
Data collection top
| High-flux four-circle diffractometer, D9 | 3217 reflections with I > 2σ(I) |
| Absorption correction: analytical: DATAP (coppens, 1970) ? | Rint = 0.026 |
| Tmin = 0.712, Tmax = 0.785 | 1 standard reflections every 50 reflections |
| 4454 measured reflections | intensity decay: none |
| 3503 independent reflections |
Refinement top
| R[F2 > 2σ(F2)] = 0.035 | All H-atom parameters refined |
| wR(F2) = 0.069 | Δρmax = 0.90 e Å−3 |
| S = 1.56 | Δρmin = −0.90 e Å−3 |
| 3493 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
| 272 parameters | Absolute structure parameter: 0.00 (999) |
| 1 restraint |
Special details top
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 on F2 for ALL reflections except for 10 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
| x | y | z | Uiso*/Ueq | ||
| Zn1 | 0.93168 (9) | 0.65599 (14) | 0.85133 (7) | 0.0071 (2) | |
| S1 | 0.8714 (2) | 0.8425 (3) | 1.02244 (14) | 0.0057 (3) | |
| S2 | 1.0157 (2) | 0.8317 (3) | 0.74579 (14) | 0.0095 (4) | |
| S3 | 0.7921 (2) | 0.4900 (3) | 0.77555 (14) | 0.0091 (4) | |
| S4 | 1.0799 (2) | 0.4974 (3) | 0.92113 (14) | 0.0082 (3) | |
| O1 | 0.84116 (10) | 0.8128 (2) | 0.92868 (7) | 0.0109 (2) | |
| O2 | 0.83581 (10) | 0.6897 (2) | 1.07213 (8) | 0.0116 (2) | |
| O3 | 0.80168 (9) | 0.9952 (2) | 1.04976 (7) | 0.0095 (2) | |
| O4 | 1.00171 (9) | 0.8759 (2) | 1.02950 (8) | 0.0110 (2) | |
| N1 | 1.14823 (7) | 0.95978 (11) | 0.87592 (5) | 0.01436 (14) | |
| H1A | 1.0836 (2) | 0.9215 (3) | 0.9182 (2) | 0.0253 (5) | |
| H1B | 1.2176 (2) | 1.0333 (4) | 0.8991 (2) | 0.0274 (5) | |
| N2 | 1.22082 (7) | 1.00052 (11) | 0.73948 (5) | 0.01465 (14) | |
| H2A | 1.2967 (2) | 1.0546 (4) | 0.7624 (2) | 0.0341 (6) | |
| H2B | 1.2128 (2) | 0.9864 (4) | 0.67448 (15) | 0.0261 (5) | |
| N3 | 0.99940 (6) | 0.35715 (11) | 0.71324 (5) | 0.01432 (14) | |
| H3A | 1.0360 (2) | 0.3830 (4) | 0.7711 (2) | 0.0310 (6) | |
| H3B | 1.0573 (2) | 0.3256 (4) | 0.6642 (2) | 0.0275 (5) | |
| N4 | 0.83700 (7) | 0.35913 (11) | 0.62231 (5) | 0.01480 (14) | |
| H4A | 0.8852 (2) | 0.2921 (4) | 0.5774 (2) | 0.0304 (5) | |
| H4B | 0.7538 (3) | 0.4028 (4) | 0.6085 (2) | 0.0375 (7) | |
| N5 | 0.89341 (6) | 0.28619 (11) | 0.96016 (5) | 0.01469 (14) | |
| H5A | 0.8493 (2) | 0.3388 (4) | 0.9094 (2) | 0.0309 (6) | |
| H5B | 0.8549 (2) | 0.1857 (3) | 0.9929 (2) | 0.0257 (5) | |
| N6 | 1.06825 (6) | 0.25250 (10) | 1.03749 (5) | 0.01260 (12) | |
| H6A | 1.0371 (2) | 0.1396 (3) | 1.0619 (2) | 0.0320 (6) | |
| H6B | 1.1540 (2) | 0.2911 (3) | 1.0501 (2) | 0.0255 (5) | |
| C1 | 1.13659 (8) | 0.93823 (13) | 0.79195 (7) | 0.0091 (2) | |
| C2 | 0.88499 (8) | 0.39664 (13) | 0.69796 (6) | 0.0091 (2) | |
| C3 | 1.00616 (8) | 0.33375 (13) | 0.97695 (6) | 0.0090 (2) |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Zn1 | 0.0073 (3) | 0.0064 (4) | 0.0077 (4) | 0.0000 (3) | −0.0008 (3) | −0.0001 (3) |
| S1 | 0.0078 (7) | 0.0043 (8) | 0.0049 (8) | 0.0010 (6) | −0.0017 (6) | 0.0000 (6) |
| S2 | 0.0099 (7) | 0.0097 (9) | 0.0088 (9) | −0.0031 (7) | −0.0013 (7) | 0.0011 (7) |
| S3 | 0.0067 (7) | 0.0128 (9) | 0.0076 (9) | 0.0001 (7) | 0.0016 (6) | −0.0028 (8) |
| S4 | 0.0069 (7) | 0.0088 (8) | 0.0090 (8) | 0.0012 (6) | 0.0015 (7) | 0.0013 (7) |
| O1 | 0.0130 (4) | 0.0117 (5) | 0.0080 (4) | 0.0041 (4) | −0.0019 (4) | −0.0020 (4) |
| O2 | 0.0112 (4) | 0.0101 (5) | 0.0134 (5) | −0.0020 (4) | −0.0017 (4) | 0.0042 (4) |
| O3 | 0.0107 (4) | 0.0089 (4) | 0.0090 (4) | 0.0001 (3) | 0.0009 (4) | −0.0012 (4) |
| O4 | 0.0075 (3) | 0.0123 (5) | 0.0131 (5) | −0.0008 (3) | −0.0007 (4) | 0.0009 (4) |
| N1 | 0.0149 (3) | 0.0194 (4) | 0.0089 (3) | −0.0073 (3) | −0.0004 (2) | −0.0010 (3) |
| H1A | 0.0261 (10) | 0.0310 (12) | 0.0189 (10) | −0.0093 (9) | 0.0036 (8) | −0.0007 (9) |
| H1B | 0.0257 (10) | 0.0341 (13) | 0.0225 (11) | −0.0123 (9) | −0.0047 (9) | −0.0044 (10) |
| N2 | 0.0131 (3) | 0.0206 (3) | 0.0103 (3) | −0.0079 (3) | 0.0008 (2) | 0.0006 (3) |
| H2A | 0.0268 (11) | 0.046 (2) | 0.0299 (13) | −0.0210 (11) | −0.0002 (10) | −0.0012 (11) |
| H2B | 0.0299 (11) | 0.0337 (13) | 0.0148 (9) | −0.0072 (10) | 0.0034 (8) | −0.0020 (9) |
| N3 | 0.0100 (2) | 0.0192 (3) | 0.0138 (3) | 0.0024 (3) | 0.0010 (2) | −0.0067 (3) |
| H3A | 0.0231 (10) | 0.044 (2) | 0.0257 (11) | 0.0078 (10) | −0.0073 (9) | −0.0131 (11) |
| H3B | 0.0183 (9) | 0.0347 (13) | 0.0296 (12) | 0.0038 (9) | 0.0044 (8) | −0.0120 (10) |
| N4 | 0.0131 (3) | 0.0217 (4) | 0.0095 (3) | 0.0005 (3) | −0.0006 (2) | −0.0055 (3) |
| H4A | 0.0296 (11) | 0.0392 (14) | 0.0225 (11) | 0.0031 (11) | 0.0041 (9) | −0.0155 (11) |
| H4B | 0.0229 (9) | 0.061 (2) | 0.0289 (13) | 0.0119 (13) | −0.0086 (10) | −0.0152 (12) |
| N5 | 0.0100 (3) | 0.0139 (3) | 0.0201 (4) | −0.0026 (2) | −0.0018 (3) | 0.0066 (3) |
| H5A | 0.0247 (10) | 0.0309 (13) | 0.0370 (14) | −0.0028 (9) | −0.0091 (10) | 0.0158 (11) |
| H5B | 0.0201 (8) | 0.0235 (10) | 0.0335 (13) | −0.0063 (8) | 0.0003 (9) | 0.0086 (10) |
| N6 | 0.0128 (2) | 0.0120 (3) | 0.0130 (3) | 0.0005 (2) | −0.0006 (2) | 0.0045 (3) |
| H6A | 0.0310 (11) | 0.0292 (12) | 0.0358 (13) | −0.0056 (10) | −0.0046 (10) | 0.0164 (11) |
| H6B | 0.0208 (8) | 0.0277 (11) | 0.0279 (12) | −0.0003 (9) | −0.0036 (9) | 0.0046 (10) |
| C1 | 0.0089 (3) | 0.0106 (4) | 0.0078 (4) | −0.0027 (3) | −0.0002 (3) | −0.0003 (3) |
| C2 | 0.0078 (3) | 0.0099 (4) | 0.0095 (4) | −0.0007 (3) | 0.0013 (3) | −0.0025 (3) |
| C3 | 0.0086 (3) | 0.0087 (4) | 0.0098 (4) | 0.0003 (3) | 0.0007 (3) | 0.0024 (3) |
Geometric parameters (Å, º) top
| Zn1—O1 | 1.980 (2) | S4—C3 | 1.738 (2) |
| Zn1—S4 | 2.317 (2) | S4—N6 | 2.622 (2) |
| Zn1—S2 | 2.324 (2) | S4—N5 | 2.700 (2) |
| Zn1—S3 | 2.328 (2) | S4—S3i | 3.263 (3) |
| Zn1—S1 | 3.099 (2) | S4—H3A | 2.544 (3) |
| S1—O2 | 1.465 (2) | N1—C1 | 1.323 (1) |
| S1—O3 | 1.473 (2) | N1—H1A | 1.016 (2) |
| S1—O4 | 1.468 (2) | N1—H1B | 1.021 (2) |
| S1—O1 | 1.514 (2) | N2—C1 | 1.329 (1) |
| S1—S4 | 3.861 (3) | N2—H2A | 1.003 (3) |
| S2—C1 | 1.727 (2) | N2—H2B | 1.021 (2) |
| S2—N2 | 2.619 (2) | N3—C2 | 1.323 (1) |
| S2—N1 | 2.689 (2) | N3—H3A | 1.006 (3) |
| S2—S3 | 3.647 (3) | N3—H3B | 1.025 (2) |
| S2—S4 | 3.823 (3) | N4—C2 | 1.323 (1) |
| S2—S3i | 3.967 (3) | N4—H4A | 1.020 (3) |
| S3—C2 | 1.742 (2) | N4—H4B | 1.003 (3) |
| S3—N4 | 2.637 (2) | N5—C3 | 1.326 (1) |
| S3—N3 | 2.693 (2) | N5—H5A | 1.013 (3) |
| S3—S4ii | 3.263 (3) | N5—H5B | 1.022 (3) |
| S3—S4 | 3.908 (3) | N6—C3 | 1.324 (1) |
| S3—S2ii | 3.967 (3) | N6—H6A | 1.012 (3) |
| S3—H5A | 2.470 (3) | N6—H6B | 1.014 (2) |
| O1—Zn1—S4 | 113.37 (8) | C3—S4—Zn1 | 106.7 (1) |
| O1—Zn1—S2 | 105.92 (8) | C3—S4—N6 | 26.69 (5) |
| S4—Zn1—S2 | 110.91 (9) | Zn1—S4—N6 | 132.09 (9) |
| O1—Zn1—S3 | 108.04 (7) | C3—S4—N5 | 24.32 (5) |
| S4—Zn1—S3 | 114.6 (1) | Zn1—S4—N5 | 83.35 (7) |
| S2—Zn1—S3 | 103.24 (9) | N6—S4—N5 | 51.01 (5) |
| O1—Zn1—S1 | 23.74 (5) | C3—S4—S3i | 134.9 (1) |
| S4—Zn1—S1 | 89.73 (7) | Zn1—S4—S3i | 99.67 (8) |
| S2—Zn1—S1 | 114.92 (8) | N6—S4—S3i | 122.42 (9) |
| S3—Zn1—S1 | 123.27 (7) | N5—S4—S3i | 136.4 (1) |
| O2—S1—O3 | 110.6 (2) | C3—S4—S2 | 139.6 (1) |
| O2—S1—O4 | 111.5 (1) | Zn1—S4—S2 | 34.61 (5) |
| O3—S1—O4 | 110.6 (2) | N6—S4—S2 | 166.17 (8) |
| O2—S1—O1 | 109.1 (2) | N5—S4—S2 | 115.27 (7) |
| O3—S1—O1 | 106.5 (1) | S3i—S4—S2 | 67.56 (7) |
| O4—S1—O1 | 108.4 (1) | C3—S4—S1 | 91.03 (9) |
| O2—S1—Zn1 | 97.9 (1) | Zn1—S4—S1 | 53.39 (6) |
| O3—S1—Zn1 | 137.1 (1) | N6—S4—S1 | 100.78 (7) |
| O4—S1—Zn1 | 86.3 (1) | N5—S4—S1 | 82.48 (6) |
| O1—S1—Zn1 | 31.77 (7) | S3i—S4—S1 | 133.82 (9) |
| O2—S1—S4 | 79.6 (1) | S2—S4—S1 | 73.38 (6) |
| O3—S1—S4 | 169.7 (1) | C3—S4—S3 | 84.05 (9) |
| O4—S1—S4 | 64.28 (9) | Zn1—S4—S3 | 32.81 (6) |
| O1—S1—S4 | 68.56 (9) | N6—S4—S3 | 110.45 (8) |
| Zn1—S1—S4 | 36.88 (4) | N5—S4—S3 | 59.92 (6) |
| C1—S2—Zn1 | 107.1 (1) | S3i—S4—S3 | 100.61 (8) |
| C1—S2—N2 | 26.77 (5) | S2—S4—S3 | 56.28 (6) |
| Zn1—S2—N2 | 131.6 (1) | S1—S4—S3 | 76.12 (6) |
| C1—S2—N1 | 24.36 (5) | C3—S4—H3A | 96.7 (1) |
| Zn1—S2—N1 | 84.32 (8) | Zn1—S4—H3A | 67.56 (8) |
| N2—S2—N1 | 51.13 (5) | N6—S4—H3A | 111.9 (1) |
| C1—S2—S3 | 144.8 (1) | N5—S4—H3A | 81.4 (1) |
| Zn1—S2—S3 | 38.41 (6) | S3i—S4—H3A | 60.71 (8) |
| N2—S2—S3 | 162.33 (9) | S2—S4—H3A | 62.89 (9) |
| N1—S2—S3 | 122.73 (8) | S1—S4—H3A | 120.03 (9) |
| C1—S2—S4 | 83.19 (9) | S3—S4—H3A | 46.14 (7) |
| Zn1—S2—S4 | 34.49 (5) | S1—O1—Zn1 | 124.5 (1) |
| N2—S2—S4 | 101.67 (7) | C1—N1—S2 | 32.56 (7) |
| N1—S2—S4 | 67.05 (6) | C1—N1—H1A | 122.3 (2) |
| S3—S2—S4 | 63.03 (6) | S2—N1—H1A | 89.8 (2) |
| C1—S2—S3i | 69.72 (8) | C1—N1—H1B | 119.5 (2) |
| Zn1—S2—S3i | 81.95 (7) | S2—N1—H1B | 151.8 (2) |
| N2—S2—S3i | 69.44 (6) | H1A—N1—H1B | 117.5 (2) |
| N1—S2—S3i | 73.89 (6) | C1—N2—S2 | 35.83 (7) |
| S3—S2—S3i | 93.12 (5) | C1—N2—H2A | 121.3 (2) |
| S4—S2—S3i | 49.49 (5) | S2—N2—H2A | 156.8 (2) |
| C2—S3—Zn1 | 100.8 (1) | C1—N2—H2B | 120.6 (2) |
| C2—S3—N4 | 26.29 (5) | S2—N2—H2B | 84.7 (2) |
| Zn1—S3—N4 | 122.98 (9) | H2A—N2—H2B | 118.0 (2) |
| C2—S3—N3 | 24.53 (5) | C2—N3—S3 | 33.12 (7) |
| Zn1—S3—N3 | 80.07 (7) | C2—N3—H3A | 119.9 (2) |
| N4—S3—N3 | 50.80 (4) | S3—N3—H3A | 86.8 (2) |
| C2—S3—S4ii | 156.6 (1) | C2—N3—H3B | 121.2 (2) |
| Zn1—S3—S4ii | 96.26 (8) | S3—N3—H3B | 152.9 (2) |
| N4—S3—S4ii | 140.76 (9) | H3A—N3—H3B | 117.5 (2) |
| N3—S3—S4ii | 150.9 (1) | C2—N4—S3 | 35.65 (6) |
| C2—S3—S2 | 79.14 (9) | C2—N4—H4A | 120.7 (2) |
| Zn1—S3—S2 | 38.34 (6) | S3—N4—H4A | 155.8 (2) |
| N4—S3—S2 | 92.01 (7) | C2—N4—H4B | 119.0 (2) |
| N3—S3—S2 | 69.68 (6) | S3—N4—H4B | 83.8 (2) |
| S4ii—S3—S2 | 123.67 (9) | H4A—N4—H4B | 120.2 (2) |
| C2—S3—S4 | 85.82 (9) | C3—N5—S4 | 32.66 (7) |
| Zn1—S3—S4 | 32.64 (5) | C3—N5—H5A | 119.7 (2) |
| N4—S3—S4 | 112.10 (7) | S4—N5—H5A | 87.1 (2) |
| N3—S3—S4 | 61.35 (5) | C3—N5—H5B | 120.3 (2) |
| S4ii—S3—S4 | 100.56 (8) | S4—N5—H5B | 152.9 (2) |
| S2—S3—S4 | 60.68 (6) | H5A—N5—H5B | 119.5 (2) |
| C2—S3—S2ii | 96.6 (1) | C3—N6—S4 | 36.11 (6) |
| Zn1—S3—S2ii | 156.26 (9) | C3—N6—H6A | 120.0 (2) |
| N4—S3—S2ii | 78.43 (6) | S4—N6—H6A | 153.9 (2) |
| N3—S3—S2ii | 112.06 (8) | C3—N6—H6B | 118.9 (2) |
| S4ii—S3—S2ii | 62.96 (6) | S4—N6—H6B | 82.9 (2) |
| S2—S3—S2ii | 164.00 (9) | H6A—N6—H6B | 119.9 (2) |
| S4—S3—S2ii | 134.82 (8) | N1—C1—N2 | 119.51 (8) |
| C2—S3—H5A | 103.7 (1) | N1—C1—S2 | 123.1 (1) |
| Zn1—S3—H5A | 70.34 (9) | N2—C1—S2 | 117.4 (1) |
| N4—S3—H5A | 122.2 (1) | N3—C2—N4 | 119.53 (8) |
| N3—S3—H5A | 84.6 (1) | N3—C2—S3 | 122.4 (1) |
| S4ii—S3—H5A | 67.24 (9) | N4—C2—S3 | 118.1 (1) |
| S2—S3—H5A | 106.0 (1) | N6—C3—N5 | 119.77 (8) |
| S4—S3—H5A | 46.34 (7) | N6—C3—S4 | 117.2 (1) |
| S2ii—S3—H5A | 89.98 (9) | N5—C3—S4 | 123.0 (1) |
| Symmetry codes: (i) x+1/2, −y+1, z; (ii) x−1/2, −y+1, z. |
Experimental details
| Crystal data | |
| Chemical formula | C3H12N6O4S4Zn |
| Mr | 389.40 |
| Crystal system, space group | Orthorhombic, Pca21 |
| Temperature (K) | 100 |
| a, b, c (Å) | 11.0616 (9), 7.7264 (6), 15.558 (1) |
| V (Å3) | 1329.7 (2) |
| Z | 4 |
| Radiation type | Neutrons, λ = 0.8369 Å |
| µ (mm−1) | 0.13 |
| Crystal size (mm) | 4.1 × 2.8 × 2.1 |
| Data collection | |
| Diffractometer | High-flux four-circle diffractometer, D9 |
| Absorption correction | Analytical: DATAP (Coppens, 1970) |
| Tmin, Tmax | 0.712, 0.785 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 4454, 3503, 3217 |
| Rint | 0.026 |
| (sin θ/λ)max (Å−1) | 0.904 |
| Refinement | |
| R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.069, 1.56 |
| No. of reflections | 3493 |
| No. of parameters | 272 |
| No. of restraints | 1 |
| H-atom treatment | All H-atom parameters refined |
| Δρmax, Δρmin (e Å−3) | 0.90, −0.90 |
| Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 |
| Absolute structure parameter | 0.00 (999) |
Computer programs: MAD (Barthelemy, 1984), RAFD9 (local program), RACER (Wilkinson et al., 1988), SHELXS86 (Sheldrick, 1990), SHELXL93 (Sheldrick, 1993), SHELXTL-Plus (Sheldrick, 1995).
