Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100009665/qa0302sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100009665/qa0302Isup2.hkl |
CCDC reference: 150381
The title compound, (I), was obtained from the reaction of trithiocyanuric acid, PPh3 and AuCN in DMF. To a solution of trithiocyanuric acid (0.5 mmol, 0.09 g) in DMF, AuCN (20 ml, 0.5 mmol, 0.12 g) and PPh3 (1 mmol, 0.26 g) were added. After stirring for 2 h, the orange solution was filtered. Ether was diffused slowly into the filtrate solution. A week later, crystals suitable for X-ray diffraction analysis were obtained.
Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; software used to prepare material for publication: SHELXTL.
[Au(C3H2N3S3)(C18H15P)3]·C3H7NO | Z = 2 |
Mr = 1233.13 | F(000) = 1244 |
Triclinic, P1 | Dx = 1.501 Mg m−3 |
a = 13.7053 (12) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.9751 (12) Å | Cell parameters from 925 reflections |
c = 14.4614 (12) Å | θ = 11.6–18.9° |
α = 80.665 (2)° | µ = 2.94 mm−1 |
β = 87.283 (2)° | T = 293 K |
γ = 87.942 (2)° | Block, colourless |
V = 2729.0 (4) Å3 | 0.25 × 0.22 × 0.20 mm |
SMART CCD diffractometer | 12409 independent reflections |
Radiation source: fine-focus sealed tube | 9513 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ω scans | θmax = 27.6°, θmin = 1.4° |
Absorption correction: multi-scan (XEMP in SHELXTL; Sheldrick, 1997) | h = −17→17 |
Tmin = 0.420, Tmax = 0.555 | k = −18→12 |
18651 measured reflections | l = −18→18 |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.113 | H-atom parameters constrained |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0602P)2] where P = (Fo2 + 2Fc2)/3 |
12409 reflections | (Δ/σ)max = 0.002 |
624 parameters | Δρmax = 1.19 e Å−3 |
0 restraints | Δρmin = −0.81 e Å−3 |
[Au(C3H2N3S3)(C18H15P)3]·C3H7NO | γ = 87.942 (2)° |
Mr = 1233.13 | V = 2729.0 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 13.7053 (12) Å | Mo Kα radiation |
b = 13.9751 (12) Å | µ = 2.94 mm−1 |
c = 14.4614 (12) Å | T = 293 K |
α = 80.665 (2)° | 0.25 × 0.22 × 0.20 mm |
β = 87.283 (2)° |
SMART CCD diffractometer | 12409 independent reflections |
Absorption correction: multi-scan (XEMP in SHELXTL; Sheldrick, 1997) | 9513 reflections with I > 2σ(I) |
Tmin = 0.420, Tmax = 0.555 | Rint = 0.035 |
18651 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | 0 restraints |
wR(F2) = 0.113 | H-atom parameters constrained |
S = 0.97 | Δρmax = 1.19 e Å−3 |
12409 reflections | Δρmin = −0.81 e Å−3 |
624 parameters |
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 | ||
Au1 | 0.758349 (14) | 0.720592 (14) | 0.700791 (13) | 0.03737 (7) | |
S1 | 0.69257 (16) | 0.65994 (12) | 0.89500 (11) | 0.0708 (5) | |
S2 | 0.43406 (14) | 0.88052 (15) | 1.04915 (14) | 0.0764 (5) | |
S3 | 0.80338 (14) | 0.89662 (16) | 1.12055 (13) | 0.0766 (5) | |
P1 | 0.65311 (9) | 0.62529 (9) | 0.62642 (9) | 0.0361 (3) | |
P2 | 0.73501 (9) | 0.89428 (9) | 0.67594 (8) | 0.0334 (3) | |
P3 | 0.92369 (9) | 0.66468 (9) | 0.73056 (9) | 0.0352 (3) | |
N1 | 0.6261 (4) | 0.8818 (4) | 1.0681 (3) | 0.0597 (13) | |
N2 | 0.7437 (4) | 0.7805 (4) | 1.0084 (3) | 0.0569 (12) | |
N3 | 0.5755 (4) | 0.7722 (4) | 0.9805 (3) | 0.0580 (13) | |
C1 | 0.6713 (5) | 0.7450 (4) | 0.9658 (4) | 0.0550 (15) | |
C2 | 0.5490 (5) | 0.8435 (4) | 1.0326 (4) | 0.0560 (15) | |
C3 | 0.7217 (4) | 0.8489 (4) | 1.0615 (4) | 0.0522 (14) | |
C11 | 0.6892 (4) | 0.6345 (3) | 0.5013 (3) | 0.0375 (11) | |
C12 | 0.7881 (4) | 0.6298 (4) | 0.4751 (4) | 0.0491 (13) | |
H12A | 0.8339 | 0.6190 | 0.5214 | 0.059* | |
C13 | 0.8197 (5) | 0.6409 (5) | 0.3823 (4) | 0.0610 (17) | |
H13A | 0.8859 | 0.6350 | 0.3663 | 0.073* | |
C14 | 0.7522 (5) | 0.6609 (5) | 0.3132 (4) | 0.0658 (18) | |
H14A | 0.7731 | 0.6711 | 0.2503 | 0.079* | |
C15 | 0.6546 (5) | 0.6655 (5) | 0.3375 (4) | 0.0663 (18) | |
H15A | 0.6092 | 0.6771 | 0.2909 | 0.080* | |
C16 | 0.6229 (4) | 0.6531 (4) | 0.4305 (4) | 0.0510 (13) | |
H16A | 0.5564 | 0.6573 | 0.4460 | 0.061* | |
C21 | 0.6509 (4) | 0.4947 (4) | 0.6687 (4) | 0.0419 (12) | |
C22 | 0.6519 (4) | 0.4277 (4) | 0.6084 (4) | 0.0460 (12) | |
H22A | 0.6567 | 0.4483 | 0.5439 | 0.055* | |
C23 | 0.6458 (5) | 0.3301 (4) | 0.6435 (5) | 0.0628 (16) | |
H23A | 0.6474 | 0.2853 | 0.6024 | 0.075* | |
C24 | 0.6373 (5) | 0.2987 (5) | 0.7375 (5) | 0.0680 (18) | |
H24A | 0.6338 | 0.2327 | 0.7605 | 0.082* | |
C25 | 0.6339 (6) | 0.3641 (5) | 0.7978 (5) | 0.086 (2) | |
H25A | 0.6261 | 0.3430 | 0.8620 | 0.103* | |
C26 | 0.6422 (6) | 0.4622 (5) | 0.7635 (4) | 0.072 (2) | |
H26A | 0.6420 | 0.5065 | 0.8052 | 0.087* | |
C31 | 0.5237 (4) | 0.6600 (4) | 0.6241 (3) | 0.0417 (12) | |
C32 | 0.4497 (4) | 0.5923 (5) | 0.6408 (4) | 0.0566 (15) | |
H32A | 0.4659 | 0.5266 | 0.6564 | 0.068* | |
C33 | 0.3526 (4) | 0.6222 (6) | 0.6344 (5) | 0.0683 (18) | |
H33A | 0.3040 | 0.5764 | 0.6455 | 0.082* | |
C34 | 0.3272 (5) | 0.7192 (6) | 0.6116 (5) | 0.072 (2) | |
H34A | 0.2617 | 0.7390 | 0.6086 | 0.087* | |
C35 | 0.3998 (5) | 0.7870 (5) | 0.5933 (5) | 0.0671 (17) | |
H35A | 0.3833 | 0.8525 | 0.5774 | 0.081* | |
C36 | 0.4972 (4) | 0.7569 (4) | 0.5989 (4) | 0.0558 (15) | |
H36A | 0.5456 | 0.8027 | 0.5854 | 0.067* | |
C41 | 0.8048 (3) | 0.9667 (3) | 0.7433 (3) | 0.0366 (10) | |
C42 | 0.7607 (4) | 1.0058 (5) | 0.8166 (4) | 0.0588 (16) | |
H42A | 0.6947 | 0.9959 | 0.8319 | 0.071* | |
C43 | 0.8135 (5) | 1.0596 (6) | 0.8678 (5) | 0.073 (2) | |
H43A | 0.7832 | 1.0847 | 0.9180 | 0.087* | |
C44 | 0.9107 (5) | 1.0763 (5) | 0.8450 (4) | 0.0630 (17) | |
H44A | 0.9457 | 1.1138 | 0.8787 | 0.076* | |
C45 | 0.9555 (4) | 1.0377 (4) | 0.7725 (4) | 0.0532 (14) | |
H45A | 1.0212 | 1.0486 | 0.7570 | 0.064* | |
C46 | 0.9034 (4) | 0.9825 (4) | 0.7223 (4) | 0.0482 (13) | |
H46A | 0.9347 | 0.9555 | 0.6737 | 0.058* | |
C51 | 0.6107 (4) | 0.9380 (4) | 0.6948 (3) | 0.0402 (11) | |
C52 | 0.5489 (4) | 0.8843 (5) | 0.7582 (4) | 0.0539 (14) | |
H52A | 0.5698 | 0.8236 | 0.7882 | 0.065* | |
C53 | 0.4551 (5) | 0.9191 (6) | 0.7787 (4) | 0.070 (2) | |
H53A | 0.4147 | 0.8824 | 0.8233 | 0.085* | |
C54 | 0.4227 (5) | 1.0061 (7) | 0.7339 (5) | 0.079 (2) | |
H54A | 0.3597 | 1.0284 | 0.7472 | 0.095* | |
C55 | 0.4817 (6) | 1.0614 (7) | 0.6692 (6) | 0.089 (2) | |
H55A | 0.4583 | 1.1206 | 0.6380 | 0.107* | |
C56 | 0.5770 (5) | 1.0295 (5) | 0.6498 (5) | 0.0681 (18) | |
H56A | 0.6180 | 1.0683 | 0.6075 | 0.082* | |
C61 | 0.7681 (3) | 0.9426 (3) | 0.5538 (3) | 0.0351 (10) | |
C62 | 0.8048 (4) | 1.0347 (4) | 0.5242 (4) | 0.0472 (13) | |
H62A | 0.8123 | 1.0764 | 0.5672 | 0.057* | |
C63 | 0.8304 (4) | 1.0643 (4) | 0.4285 (4) | 0.0529 (14) | |
H63A | 0.8555 | 1.1256 | 0.4087 | 0.063* | |
C64 | 0.8190 (4) | 1.0045 (5) | 0.3655 (4) | 0.0542 (14) | |
H64A | 0.8362 | 1.0251 | 0.3026 | 0.065* | |
C65 | 0.7824 (4) | 0.9144 (4) | 0.3929 (4) | 0.0551 (15) | |
H65A | 0.7745 | 0.8738 | 0.3490 | 0.066* | |
C66 | 0.7570 (4) | 0.8837 (4) | 0.4869 (4) | 0.0473 (13) | |
H66A | 0.7320 | 0.8223 | 0.5052 | 0.057* | |
C71 | 0.9475 (4) | 0.5397 (4) | 0.7855 (3) | 0.0396 (11) | |
C72 | 0.9010 (6) | 0.4657 (5) | 0.7572 (5) | 0.082 (2) | |
H72A | 0.8540 | 0.4797 | 0.7122 | 0.099* | |
C73 | 0.9223 (7) | 0.3698 (5) | 0.7941 (6) | 0.098 (3) | |
H73A | 0.8907 | 0.3205 | 0.7725 | 0.118* | |
C74 | 0.9888 (6) | 0.3471 (5) | 0.8614 (5) | 0.080 (2) | |
H74A | 1.0033 | 0.2826 | 0.8856 | 0.095* | |
C75 | 1.0331 (6) | 0.4189 (6) | 0.8925 (6) | 0.092 (3) | |
H75A | 1.0789 | 0.4041 | 0.9386 | 0.111* | |
C76 | 1.0114 (5) | 0.5154 (5) | 0.8565 (5) | 0.078 (2) | |
H76A | 1.0406 | 0.5644 | 0.8810 | 0.093* | |
C81 | 0.9945 (4) | 0.7358 (3) | 0.7982 (3) | 0.0376 (11) | |
C82 | 0.9465 (4) | 0.7756 (4) | 0.8713 (4) | 0.0502 (13) | |
H82A | 0.8801 | 0.7659 | 0.8843 | 0.060* | |
C83 | 0.9967 (5) | 0.8286 (5) | 0.9235 (4) | 0.0650 (17) | |
H83A | 0.9646 | 0.8554 | 0.9718 | 0.078* | |
C84 | 1.0931 (6) | 0.8422 (5) | 0.9050 (5) | 0.070 (2) | |
H84A | 1.1267 | 0.8785 | 0.9410 | 0.084* | |
C85 | 1.1427 (5) | 0.8038 (5) | 0.8347 (5) | 0.0683 (19) | |
H85A | 1.2092 | 0.8137 | 0.8233 | 0.082* | |
C86 | 1.0925 (4) | 0.7499 (4) | 0.7805 (4) | 0.0523 (14) | |
H86A | 1.1254 | 0.7234 | 0.7324 | 0.063* | |
C91 | 0.9932 (3) | 0.6753 (4) | 0.6186 (3) | 0.0360 (11) | |
C92 | 0.9778 (4) | 0.7586 (4) | 0.5543 (4) | 0.0474 (13) | |
H92A | 0.9339 | 0.8064 | 0.5697 | 0.057* | |
C93 | 1.0268 (4) | 0.7721 (5) | 0.4670 (4) | 0.0569 (15) | |
H93A | 1.0149 | 0.8281 | 0.4243 | 0.068* | |
C94 | 1.1068 (5) | 0.6213 (6) | 0.5073 (5) | 0.084 (2) | |
H94A | 1.1502 | 0.5736 | 0.4911 | 0.100* | |
C95 | 1.0918 (5) | 0.7038 (6) | 0.4442 (5) | 0.071 (2) | |
H95A | 1.1258 | 0.7129 | 0.3864 | 0.086* | |
C96 | 1.0593 (5) | 0.6069 (5) | 0.5942 (4) | 0.0651 (17) | |
H96A | 1.0721 | 0.5507 | 0.6364 | 0.078* | |
O1 | 0.5867 (7) | 0.3182 (8) | 1.0733 (7) | 0.177 (4)* | |
N5 | 0.6814 (7) | 0.4348 (6) | 1.0853 (6) | 0.115 (3)* | |
C4 | 0.5937 (14) | 0.4033 (14) | 1.0957 (12) | 0.218 (7)* | |
H4A | 0.5408 | 0.4383 | 1.1171 | 0.262* | |
C5 | 0.6828 (11) | 0.5166 (12) | 1.1291 (11) | 0.209 (7)* | |
H5A | 0.6238 | 0.5207 | 1.1668 | 0.313* | |
H5B | 0.6876 | 0.5737 | 1.0824 | 0.313* | |
H5C | 0.7380 | 0.5117 | 1.1682 | 0.313* | |
C6 | 0.7652 (8) | 0.4136 (9) | 1.0233 (8) | 0.150 (4)* | |
H6A | 0.7521 | 0.3576 | 0.9956 | 0.225* | |
H6B | 0.8228 | 0.4010 | 1.0591 | 0.225* | |
H6C | 0.7753 | 0.4683 | 0.9746 | 0.225* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au1 | 0.03814 (11) | 0.03568 (11) | 0.03867 (11) | −0.00120 (7) | −0.00544 (7) | −0.00597 (8) |
S1 | 0.1250 (16) | 0.0460 (9) | 0.0424 (8) | −0.0118 (9) | 0.0154 (9) | −0.0130 (7) |
S2 | 0.0638 (11) | 0.0846 (13) | 0.0790 (12) | −0.0058 (9) | 0.0142 (9) | −0.0120 (10) |
S3 | 0.0707 (11) | 0.0997 (15) | 0.0691 (11) | −0.0110 (10) | −0.0039 (9) | −0.0406 (11) |
P1 | 0.0377 (7) | 0.0351 (7) | 0.0371 (7) | −0.0027 (5) | −0.0045 (5) | −0.0093 (6) |
P2 | 0.0350 (6) | 0.0327 (6) | 0.0333 (6) | 0.0003 (5) | −0.0033 (5) | −0.0077 (5) |
P3 | 0.0357 (6) | 0.0354 (7) | 0.0346 (6) | 0.0003 (5) | −0.0047 (5) | −0.0056 (5) |
N1 | 0.068 (3) | 0.056 (3) | 0.060 (3) | −0.003 (3) | −0.004 (3) | −0.024 (3) |
N2 | 0.069 (3) | 0.055 (3) | 0.049 (3) | −0.004 (2) | 0.009 (2) | −0.017 (2) |
N3 | 0.079 (4) | 0.052 (3) | 0.044 (3) | −0.012 (3) | 0.002 (2) | −0.009 (2) |
C1 | 0.088 (5) | 0.042 (3) | 0.033 (3) | −0.004 (3) | 0.011 (3) | −0.003 (2) |
C2 | 0.067 (4) | 0.052 (4) | 0.046 (3) | −0.009 (3) | 0.008 (3) | 0.001 (3) |
C3 | 0.061 (4) | 0.055 (4) | 0.042 (3) | −0.003 (3) | 0.002 (3) | −0.010 (3) |
C11 | 0.049 (3) | 0.029 (2) | 0.036 (3) | −0.004 (2) | −0.002 (2) | −0.009 (2) |
C12 | 0.050 (3) | 0.051 (3) | 0.051 (3) | −0.007 (2) | −0.003 (2) | −0.017 (3) |
C13 | 0.068 (4) | 0.062 (4) | 0.058 (4) | −0.014 (3) | 0.019 (3) | −0.027 (3) |
C14 | 0.093 (5) | 0.061 (4) | 0.045 (3) | −0.011 (4) | 0.019 (3) | −0.016 (3) |
C15 | 0.089 (5) | 0.070 (4) | 0.040 (3) | 0.005 (4) | −0.014 (3) | −0.010 (3) |
C16 | 0.049 (3) | 0.063 (4) | 0.043 (3) | 0.002 (3) | −0.006 (2) | −0.013 (3) |
C21 | 0.043 (3) | 0.040 (3) | 0.043 (3) | −0.005 (2) | −0.008 (2) | −0.006 (2) |
C22 | 0.058 (3) | 0.039 (3) | 0.042 (3) | −0.005 (2) | −0.001 (2) | −0.009 (2) |
C23 | 0.075 (4) | 0.042 (3) | 0.074 (4) | −0.006 (3) | 0.001 (3) | −0.017 (3) |
C24 | 0.087 (5) | 0.038 (3) | 0.077 (5) | −0.015 (3) | −0.014 (4) | 0.003 (3) |
C25 | 0.142 (7) | 0.060 (5) | 0.054 (4) | −0.026 (5) | −0.015 (4) | 0.006 (4) |
C26 | 0.130 (6) | 0.048 (4) | 0.042 (3) | −0.022 (4) | −0.014 (4) | −0.008 (3) |
C31 | 0.040 (3) | 0.054 (3) | 0.034 (3) | −0.003 (2) | −0.002 (2) | −0.015 (2) |
C32 | 0.048 (3) | 0.065 (4) | 0.054 (3) | −0.007 (3) | 0.003 (3) | −0.003 (3) |
C33 | 0.043 (3) | 0.089 (5) | 0.069 (4) | −0.013 (3) | 0.003 (3) | −0.002 (4) |
C34 | 0.044 (4) | 0.111 (6) | 0.066 (4) | 0.009 (4) | 0.000 (3) | −0.028 (4) |
C35 | 0.061 (4) | 0.071 (4) | 0.075 (4) | 0.018 (3) | −0.016 (3) | −0.025 (4) |
C36 | 0.054 (3) | 0.054 (4) | 0.064 (4) | −0.005 (3) | −0.017 (3) | −0.020 (3) |
C41 | 0.041 (3) | 0.034 (3) | 0.036 (3) | 0.003 (2) | −0.009 (2) | −0.008 (2) |
C42 | 0.049 (3) | 0.081 (4) | 0.056 (3) | 0.000 (3) | −0.007 (3) | −0.036 (3) |
C43 | 0.070 (4) | 0.101 (6) | 0.061 (4) | −0.011 (4) | 0.000 (3) | −0.049 (4) |
C44 | 0.062 (4) | 0.068 (4) | 0.067 (4) | −0.006 (3) | −0.019 (3) | −0.028 (3) |
C45 | 0.042 (3) | 0.059 (4) | 0.060 (4) | −0.010 (3) | −0.009 (3) | −0.011 (3) |
C46 | 0.048 (3) | 0.056 (3) | 0.043 (3) | 0.002 (2) | −0.005 (2) | −0.016 (3) |
C51 | 0.038 (3) | 0.047 (3) | 0.038 (3) | 0.006 (2) | −0.006 (2) | −0.015 (2) |
C52 | 0.048 (3) | 0.071 (4) | 0.043 (3) | 0.000 (3) | −0.001 (2) | −0.013 (3) |
C53 | 0.051 (4) | 0.116 (6) | 0.047 (4) | −0.004 (4) | 0.003 (3) | −0.022 (4) |
C54 | 0.051 (4) | 0.136 (7) | 0.056 (4) | 0.035 (4) | −0.013 (3) | −0.038 (5) |
C55 | 0.070 (5) | 0.109 (7) | 0.089 (6) | 0.046 (5) | −0.019 (4) | −0.025 (5) |
C56 | 0.061 (4) | 0.059 (4) | 0.079 (5) | 0.013 (3) | −0.002 (3) | −0.001 (4) |
C61 | 0.038 (3) | 0.033 (3) | 0.035 (2) | 0.0024 (19) | −0.004 (2) | −0.008 (2) |
C62 | 0.054 (3) | 0.043 (3) | 0.045 (3) | −0.006 (2) | −0.003 (2) | −0.007 (3) |
C63 | 0.055 (3) | 0.047 (3) | 0.052 (3) | −0.008 (3) | −0.006 (3) | 0.009 (3) |
C64 | 0.057 (3) | 0.066 (4) | 0.036 (3) | 0.007 (3) | 0.002 (2) | 0.000 (3) |
C65 | 0.072 (4) | 0.055 (4) | 0.038 (3) | 0.007 (3) | −0.009 (3) | −0.007 (3) |
C66 | 0.059 (3) | 0.040 (3) | 0.045 (3) | −0.006 (2) | −0.006 (2) | −0.010 (2) |
C71 | 0.046 (3) | 0.037 (3) | 0.036 (3) | 0.000 (2) | −0.003 (2) | −0.004 (2) |
C72 | 0.123 (6) | 0.047 (4) | 0.079 (5) | −0.010 (4) | −0.049 (5) | 0.000 (4) |
C73 | 0.168 (9) | 0.036 (4) | 0.095 (6) | −0.014 (4) | −0.051 (6) | −0.007 (4) |
C74 | 0.120 (6) | 0.045 (4) | 0.069 (4) | 0.004 (4) | −0.013 (4) | 0.006 (3) |
C75 | 0.110 (6) | 0.061 (5) | 0.100 (6) | −0.006 (4) | −0.050 (5) | 0.018 (4) |
C76 | 0.094 (5) | 0.046 (4) | 0.091 (5) | −0.012 (3) | −0.044 (4) | 0.010 (4) |
C81 | 0.045 (3) | 0.032 (3) | 0.035 (3) | −0.001 (2) | −0.009 (2) | −0.002 (2) |
C82 | 0.063 (4) | 0.049 (3) | 0.040 (3) | 0.001 (3) | −0.016 (3) | −0.008 (3) |
C83 | 0.091 (5) | 0.061 (4) | 0.045 (3) | 0.003 (4) | −0.026 (3) | −0.011 (3) |
C84 | 0.099 (6) | 0.060 (4) | 0.055 (4) | −0.018 (4) | −0.037 (4) | −0.006 (3) |
C85 | 0.061 (4) | 0.076 (5) | 0.065 (4) | −0.031 (3) | −0.020 (3) | 0.008 (4) |
C86 | 0.051 (3) | 0.056 (4) | 0.048 (3) | −0.012 (3) | −0.008 (3) | 0.002 (3) |
C91 | 0.026 (2) | 0.044 (3) | 0.038 (3) | −0.0006 (19) | −0.0035 (19) | −0.009 (2) |
C92 | 0.042 (3) | 0.053 (3) | 0.047 (3) | 0.003 (2) | 0.000 (2) | −0.008 (3) |
C93 | 0.060 (4) | 0.066 (4) | 0.042 (3) | −0.012 (3) | −0.004 (3) | 0.001 (3) |
C94 | 0.077 (5) | 0.091 (6) | 0.083 (5) | 0.014 (4) | 0.036 (4) | −0.029 (5) |
C95 | 0.068 (4) | 0.094 (6) | 0.054 (4) | −0.018 (4) | 0.021 (3) | −0.020 (4) |
C96 | 0.071 (4) | 0.059 (4) | 0.061 (4) | 0.013 (3) | 0.012 (3) | −0.003 (3) |
Au1—P1 | 2.4001 (12) | C41—C42 | 1.375 (7) |
Au1—P3 | 2.4056 (13) | C41—C46 | 1.388 (7) |
Au1—P2 | 2.4074 (13) | C42—C43 | 1.382 (8) |
Au1—S1 | 2.9090 (15) | C43—C44 | 1.376 (9) |
S1—C1 | 1.699 (6) | C44—C45 | 1.365 (8) |
S2—C2 | 1.659 (7) | C45—C46 | 1.380 (7) |
S3—C3 | 1.660 (6) | C51—C52 | 1.368 (7) |
P1—C31 | 1.822 (5) | C51—C56 | 1.410 (8) |
P1—C21 | 1.829 (5) | C52—C53 | 1.394 (9) |
P1—C11 | 1.839 (5) | C53—C54 | 1.352 (10) |
P2—C51 | 1.812 (5) | C54—C55 | 1.366 (11) |
P2—C61 | 1.828 (5) | C55—C56 | 1.395 (9) |
P2—C41 | 1.835 (5) | C61—C66 | 1.385 (7) |
P3—C91 | 1.826 (5) | C61—C62 | 1.394 (7) |
P3—C71 | 1.822 (5) | C62—C63 | 1.410 (8) |
P3—C81 | 1.833 (5) | C63—C64 | 1.351 (8) |
N1—C2 | 1.358 (8) | C64—C65 | 1.364 (8) |
N1—C3 | 1.378 (8) | C65—C66 | 1.388 (7) |
N2—C3 | 1.337 (7) | C71—C72 | 1.362 (8) |
N2—C1 | 1.342 (8) | C71—C76 | 1.373 (8) |
N3—C2 | 1.373 (8) | C72—C73 | 1.386 (9) |
N3—C1 | 1.371 (8) | C73—C74 | 1.358 (10) |
C11—C16 | 1.388 (7) | C74—C75 | 1.340 (10) |
C11—C12 | 1.391 (7) | C75—C76 | 1.392 (10) |
C12—C13 | 1.376 (8) | C81—C86 | 1.371 (7) |
C13—C14 | 1.382 (9) | C81—C82 | 1.400 (7) |
C14—C15 | 1.370 (9) | C82—C83 | 1.365 (8) |
C15—C16 | 1.378 (8) | C83—C84 | 1.350 (9) |
C21—C26 | 1.374 (8) | C84—C85 | 1.366 (10) |
C21—C22 | 1.378 (7) | C85—C86 | 1.392 (8) |
C22—C23 | 1.380 (8) | C91—C96 | 1.369 (8) |
C23—C24 | 1.360 (9) | C91—C92 | 1.384 (7) |
C24—C25 | 1.359 (10) | C92—C93 | 1.389 (8) |
C25—C26 | 1.387 (9) | C93—C95 | 1.351 (9) |
C31—C36 | 1.385 (8) | C94—C95 | 1.365 (10) |
C31—C32 | 1.398 (7) | C94—C96 | 1.376 (9) |
C32—C33 | 1.384 (9) | O1—C4 | 1.290 (18) |
C33—C34 | 1.378 (10) | N5—C4 | 1.289 (18) |
C34—C35 | 1.385 (10) | N5—C5 | 1.395 (16) |
C35—C36 | 1.387 (8) | N5—C6 | 1.475 (13) |
P1—Au1—P3 | 119.69 (4) | C34—C33—C32 | 120.6 (6) |
P1—Au1—P2 | 118.99 (4) | C33—C34—C35 | 119.5 (6) |
P3—Au1—P2 | 114.48 (4) | C36—C35—C34 | 119.9 (7) |
P1—Au1—S1 | 99.14 (5) | C31—C36—C35 | 121.2 (6) |
P3—Au1—S1 | 92.84 (5) | C42—C41—C46 | 118.5 (5) |
P2—Au1—S1 | 104.21 (4) | C42—C41—P2 | 120.6 (4) |
C1—S1—Au1 | 119.29 (19) | C46—C41—P2 | 120.9 (4) |
C31—P1—C21 | 102.6 (2) | C41—C42—C43 | 120.6 (6) |
C31—P1—C11 | 102.9 (2) | C44—C43—C42 | 120.3 (6) |
C21—P1—C11 | 104.2 (2) | C45—C44—C43 | 119.7 (5) |
C31—P1—Au1 | 117.55 (17) | C44—C45—C46 | 120.1 (5) |
C21—P1—Au1 | 117.98 (16) | C45—C46—C41 | 120.8 (5) |
C11—P1—Au1 | 109.83 (15) | C52—C51—C56 | 118.3 (5) |
C51—P2—C61 | 105.2 (2) | C52—C51—P2 | 119.9 (4) |
C51—P2—C41 | 102.4 (2) | C56—C51—P2 | 121.6 (4) |
C61—P2—C41 | 103.9 (2) | C51—C52—C53 | 121.1 (6) |
C51—P2—Au1 | 115.39 (17) | C54—C53—C52 | 120.1 (7) |
C61—P2—Au1 | 109.16 (16) | C53—C54—C55 | 120.6 (7) |
C41—P2—Au1 | 119.35 (16) | C54—C55—C56 | 120.3 (7) |
C91—P3—C71 | 104.0 (2) | C55—C56—C51 | 119.5 (7) |
C91—P3—C81 | 102.8 (2) | C66—C61—C62 | 118.1 (5) |
C71—P3—C81 | 103.6 (2) | C66—C61—P2 | 118.0 (4) |
C91—P3—Au1 | 108.46 (15) | C62—C61—P2 | 123.9 (4) |
C71—P3—Au1 | 119.58 (16) | C61—C62—C63 | 119.5 (5) |
C81—P3—Au1 | 116.50 (17) | C64—C63—C62 | 120.6 (5) |
C2—N1—C3 | 125.1 (5) | C63—C64—C65 | 120.8 (5) |
C3—N2—C1 | 118.7 (5) | C64—C65—C66 | 119.5 (5) |
C2—N3—C1 | 121.9 (5) | C65—C66—C61 | 121.5 (5) |
N2—C1—N3 | 121.6 (5) | C72—C71—C76 | 117.0 (5) |
N2—C1—S1 | 122.1 (5) | C72—C71—P3 | 120.3 (4) |
N3—C1—S1 | 116.2 (5) | C76—C71—P3 | 122.6 (4) |
N1—C2—N3 | 113.6 (6) | C71—C72—C73 | 121.3 (6) |
N1—C2—S2 | 123.3 (5) | C74—C73—C72 | 120.7 (7) |
N3—C2—S2 | 123.1 (5) | C75—C74—C73 | 119.0 (7) |
N2—C3—N1 | 118.6 (5) | C74—C75—C76 | 120.6 (7) |
N2—C3—S3 | 123.7 (5) | C71—C76—C75 | 121.2 (6) |
N1—C3—S3 | 117.8 (4) | C86—C81—C82 | 119.2 (5) |
C16—C11—C12 | 117.8 (5) | C86—C81—P3 | 122.3 (4) |
C16—C11—P1 | 123.1 (4) | C82—C81—P3 | 118.4 (4) |
C12—C11—P1 | 118.9 (4) | C83—C82—C81 | 120.2 (6) |
C13—C12—C11 | 121.5 (5) | C84—C83—C82 | 119.9 (6) |
C12—C13—C14 | 119.5 (6) | C83—C84—C85 | 121.7 (6) |
C15—C14—C13 | 119.8 (6) | C84—C85—C86 | 119.3 (6) |
C14—C15—C16 | 120.6 (6) | C81—C86—C85 | 119.8 (6) |
C15—C16—C11 | 120.7 (6) | C96—C91—C92 | 118.0 (5) |
C26—C21—C22 | 118.7 (5) | C96—C91—P3 | 124.6 (4) |
C26—C21—P1 | 119.1 (4) | C92—C91—P3 | 117.4 (4) |
C22—C21—P1 | 122.2 (4) | C91—C92—C93 | 121.1 (5) |
C21—C22—C23 | 120.1 (5) | C95—C93—C92 | 120.1 (6) |
C24—C23—C22 | 120.8 (6) | C95—C94—C96 | 121.8 (7) |
C23—C24—C25 | 119.8 (6) | C93—C95—C94 | 119.0 (6) |
C24—C25—C26 | 120.0 (6) | C91—C96—C94 | 120.0 (6) |
C21—C26—C25 | 120.6 (6) | C4—N5—C5 | 107.3 (13) |
C36—C31—C32 | 118.3 (5) | C4—N5—C6 | 132.0 (13) |
C36—C31—P1 | 118.8 (4) | C5—N5—C6 | 119.1 (11) |
C32—C31—P1 | 122.8 (5) | N5—C4—O1 | 113.3 (17) |
C33—C32—C31 | 120.5 (6) |
Experimental details
Crystal data | |
Chemical formula | [Au(C3H2N3S3)(C18H15P)3]·C3H7NO |
Mr | 1233.13 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 13.7053 (12), 13.9751 (12), 14.4614 (12) |
α, β, γ (°) | 80.665 (2), 87.283 (2), 87.942 (2) |
V (Å3) | 2729.0 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.94 |
Crystal size (mm) | 0.25 × 0.22 × 0.20 |
Data collection | |
Diffractometer | SMART CCD diffractometer |
Absorption correction | Multi-scan (XEMP in SHELXTL; Sheldrick, 1997) |
Tmin, Tmax | 0.420, 0.555 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18651, 12409, 9513 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.651 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.113, 0.97 |
No. of reflections | 12409 |
No. of parameters | 624 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.19, −0.81 |
Computer programs: SMART (Siemens, 1994), SMART, SAINT, SHELXTL (Sheldrick, 1997), SHELXTL.
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There has been growing interest in the study of CuI, AgI and AuI complexes, and in particular polynuclear systems; this stems from the tendency of these metal ions to form clusters and aggregates as a result of weak metal–metal interactions (Mingos, 1976; Schmidbaur, 1995) and the recent demonstration that a number of these aggregates exhibit rich luminescence behaviour (Vickery et al., 1997; Yam et al., 1999). Till now, AuI–sulfido complexes are comparatively rare (Canales et al., 1994). Recently, an interesting example was found in studies of trigold(I) complexes of trithiocyanuric acid, in which an unexpected reaction led to formation of an interesting sheet structure through multiple intermolecular Au···Au-bonded self-assembly (William et al., 1999). Also by use of AuI, PPh3 and trithiocyanuric acid, we obtained a different product, (4,6-Dimercapto-1,3,5-triazine-2-thiolato-S2)tris(triphenylphosphine- P)gold(I) dimethylformamide (DMF) solvate, (I), including a DMF molecule, one AuI atom, one trithiocyanurate ligand and three PPh3 ligands. In the crystal structure, only one thiolate of the trithiocyanuric acid has been coordinated to the AuI atom and each AuI is coordinated by one thiolate group of the trithiocyanurate ligand and three P atoms of the PPh3 groups, giving a tetrahedral coordination. The S—Au distance is 2.909 (2) Å, which is much longer than the normal S—Au distance. and the P—Au distances fall in the range 2.400 (14)–2.4074 (13) Å. The S—Au—P angles are 92.81 (6), 99.17 (6) and 104.21 (5)°, and the P—Au—P angles are 114.46 (5), 119.04 (5) and 119.66 (5)°. Thus, the geometry is distorted tetrahedral.