Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806001577/xu6095sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806001577/xu6095Isup2.hkl |
CCDC reference: 298707
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXTL.
(NH4N)[Au(NCS)2] | F(000) = 1184 |
Mr = 331.17 | Dx = 3.240 Mg m−3 |
Monoclinic, C2/c | Melting point: 164 ° with decomposition K |
Hall symbol: -C 2yc | Cu Kα radiation, λ = 1.54184 Å |
a = 12.9665 (2) Å | Cell parameters from 3756 reflections |
b = 6.3132 (1) Å | θ = 5.3–67.7° |
c = 17.6643 (3) Å | µ = 45.69 mm−1 |
β = 110.122 (1)° | T = 150 K |
V = 1357.74 (4) Å3 | Rod, colorless |
Z = 8 | 0.11 × 0.04 × 0.03 mm |
SMART6000 CCD diffractometer | 1209 independent reflections |
Radiation source: fine-focus sealed tube | 1123 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
Detector resolution: 0.83 pixels mm-1 | θmax = 67.7°, θmin = 5.3° |
ω scans | h = −15→15 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −6→7 |
Tmin = 0.061, Tmax = 0.256 | l = −21→21 |
5457 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.059 | w = 1/[σ2(Fo2) + (0.033P)2 + 4.3348P] where P = (Fo2 + 2Fc2)/3 |
S = 1.16 | (Δ/σ)max < 0.001 |
1209 reflections | Δρmax = 0.97 e Å−3 |
75 parameters | Δρmin = −1.58 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.000284 (16) |
Experimental. A suitable crystal was mounted on the tip of a glass fiber with paratone-N. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 σ(I). Note that the absorption correction parameters Tmin and Tmax also reflect beam corrections, etc. As a result, the numerical values for Tmin and Tmax may differ from expected values based solely absorption effects and crystal size. |
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 | ||
N3 | 0.3265 (3) | 0.4904 (6) | 0.4413 (2) | 0.0247 (8) | |
H1 | 0.3677 | 0.6016 | 0.4700 | 0.037* | |
H2 | 0.3795 | 0.3984 | 0.4481 | 0.037* | |
H3 | 0.2768 | 0.4585 | 0.4629 | 0.037* | |
H4 | 0.2885 | 0.5604 | 0.3989 | 0.037* | |
Au1 | 0.5000 | 0.32757 (4) | 0.2500 | 0.01534 (14) | |
Au2 | 0.5000 | 0.83005 (4) | 0.2500 | 0.01348 (14) | |
S1 | 0.68661 (9) | 0.31698 (17) | 0.27506 (6) | 0.0211 (3) | |
S2 | 0.51549 (10) | 0.80341 (17) | 0.38350 (6) | 0.0226 (3) | |
N1 | 0.7635 (3) | 0.5370 (7) | 0.4234 (3) | 0.0287 (9) | |
N2 | 0.5183 (3) | 1.2261 (6) | 0.4365 (2) | 0.0235 (8) | |
C1 | 0.7301 (4) | 0.4525 (7) | 0.3623 (3) | 0.0190 (9) | |
C2 | 0.5166 (3) | 1.0562 (7) | 0.4128 (2) | 0.0145 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
N3 | 0.028 (2) | 0.021 (2) | 0.0213 (19) | 0.0007 (16) | 0.0028 (16) | 0.0032 (16) |
Au1 | 0.0198 (2) | 0.0153 (2) | 0.00869 (19) | 0.000 | 0.00201 (12) | 0.000 |
Au2 | 0.01860 (19) | 0.0152 (2) | 0.00682 (18) | 0.000 | 0.00463 (12) | 0.000 |
S1 | 0.0214 (5) | 0.0229 (6) | 0.0191 (6) | 0.0008 (4) | 0.0070 (4) | −0.0029 (4) |
S2 | 0.0431 (7) | 0.0182 (5) | 0.0087 (5) | 0.0062 (5) | 0.0117 (5) | 0.0027 (4) |
N1 | 0.021 (2) | 0.034 (2) | 0.026 (2) | 0.0022 (17) | 0.0003 (18) | −0.0086 (18) |
N2 | 0.036 (2) | 0.025 (2) | 0.0115 (18) | 0.0018 (17) | 0.0104 (16) | −0.0011 (16) |
C1 | 0.011 (2) | 0.019 (2) | 0.026 (3) | 0.0030 (15) | 0.0039 (18) | 0.0024 (18) |
C2 | 0.017 (2) | 0.022 (2) | 0.0049 (19) | 0.0020 (15) | 0.0039 (16) | 0.0012 (16) |
N3—H1 | 0.9211 | Au1—Au2 | 3.1723 (3) |
N3—H2 | 0.8757 | Au2—S2 | 2.3030 (10) |
N3—H3 | 0.8780 | S1—C1 | 1.680 (5) |
N3—H4 | 0.8635 | S2—C2 | 1.676 (4) |
Au1—S1 | 2.3062 (11) | N1—C1 | 1.148 (6) |
Au1—Au2i | 3.1409 (3) | N2—C2 | 1.149 (6) |
H1—N3—H2 | 98.7 | Au2i—Au1—Au2 | 180.0 |
H1—N3—H3 | 108.0 | S2ii—Au2—S2 | 171.63 (5) |
H2—N3—H3 | 116.6 | S2—Au2—Au1iii | 94.19 (3) |
H1—N3—H4 | 97.9 | C1—S1—Au1 | 99.22 (15) |
H2—N3—H4 | 130.2 | C2—S2—Au2 | 103.59 (15) |
H3—N3—H4 | 102.0 | N1—C1—S1 | 176.6 (4) |
S1—Au1—S1ii | 176.68 (5) | N2—C2—S2 | 176.8 (4) |
S1—Au1—Au2i | 88.34 (3) | ||
Au2i—Au1—S1—C1 | −121.37 (16) | Au1iii—Au2—S2—C2 | 1.00 (16) |
Au2—Au1—S1—C1 | 58.63 (16) |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y, −z+1/2; (iii) x, y+1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H1···N2iv | 0.92 | 2.10 | 2.987 (6) | 161 |
N3—H2···N2i | 0.88 | 2.17 | 3.020 (6) | 163 |
N3—H3···N1v | 0.88 | 2.24 | 3.004 (6) | 145 |
Symmetry codes: (i) x, y−1, z; (iv) −x+1, −y+2, −z+1; (v) −x+1, −y+1, −z+1. |