Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806024354/xu2066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806024354/xu2066Isup2.hkl |
CCDC reference: 613866
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.016 Å
- R factor = 0.058
- wR factor = 0.158
- Data-to-parameter ratio = 16.0
checkCIF/PLATON results
No syntax errors found
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.103 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.10 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.50 Ratio PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.68 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 16
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus and XPREP (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Au2Fe(C38H37NP2)(NCS)2] | Z = 2 |
Mr = 1135.57 | F(000) = 1088 |
Triclinic, P1 | Dx = 1.955 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 9.021 (5) Å | Cell parameters from 1018 reflections |
b = 13.397 (5) Å | θ = 2.8–25.0° |
c = 16.684 (5) Å | µ = 8.18 mm−1 |
α = 89.956 (5)° | T = 293 K |
β = 82.946 (5)° | Needle, orange |
γ = 74.740 (5)° | 0.37 × 0.14 × 0.08 mm |
V = 1929.5 (14) Å3 |
Bruker SMART 1K CCD diffractometer | 6743 independent reflections |
Radiation source: fine-focus sealed tube | 5497 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.103 |
ω scans | θmax = 25.0°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −10→10 |
Tmin = 0.260, Tmax = 0.519 | k = −15→9 |
10576 measured reflections | l = −18→19 |
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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.158 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.1108P)2] where P = (Fo2 + 2Fc2)/3 |
6743 reflections | (Δ/σ)max = 0.001 |
421 parameters | Δρmax = 3.11 e Å−3 |
0 restraints | Δρmin = −3.23 e Å−3 |
Experimental. The intensity data were collected on a Bruker SMART CCD 1 K diffractometer using an exposure time of 10 s/frame. A total of 512 frames were collected with a frame width of 0.3° covering up to θ = 25° with 99.3% completeness accomplished. The first 50 frames were recollected at the end of the data collection to check for decay; none was found. 1H NMR (CDCl3, 300 MHz): 0.81 (d), 1.53 (s), 3.84–4.97 (m), 7.34–7.75 (m); 31P{1H} NMR (CDCl3, 121.5 MHz): 31.53 (s), 32.94 (s); IR (KBr, ν (SCN), cm-1): 2117(s). |
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 | 0.57622 (4) | 0.43166 (3) | 0.34232 (2) | 0.03540 (15) | |
Au2 | −0.09847 (4) | 0.88294 (3) | 0.14743 (2) | 0.04004 (15) | |
P1 | 0.4442 (3) | 0.38373 (17) | 0.24873 (14) | 0.0295 (5) | |
P2 | 0.0149 (3) | 0.88233 (18) | 0.26104 (15) | 0.0357 (5) | |
S1 | 0.7079 (4) | 0.4934 (3) | 0.43422 (18) | 0.0550 (7) | |
S2 | −0.2204 (4) | 0.8932 (2) | 0.03239 (19) | 0.0595 (8) | |
N1 | 0.5661 (17) | 0.7065 (11) | 0.4167 (9) | 0.102 (5) | |
N2 | −0.1186 (15) | 0.6939 (10) | −0.0395 (7) | 0.081 (4) | |
N3 | 0.6680 (8) | 0.5041 (6) | 0.1559 (5) | 0.0377 (18) | |
Fe | 0.18448 (13) | 0.62004 (9) | 0.24569 (7) | 0.0286 (3) | |
C1 | 0.6238 (15) | 0.6193 (11) | 0.4229 (8) | 0.064 (3) | |
C11 | 0.5637 (10) | 0.2922 (6) | 0.1716 (6) | 0.033 (2) | |
C12 | 0.7195 (11) | 0.2511 (8) | 0.1806 (6) | 0.044 (2) | |
H12 | 0.7592 | 0.2699 | 0.2254 | 0.053* | |
C13 | 0.8160 (13) | 0.1810 (9) | 0.1217 (7) | 0.056 (3) | |
H13 | 0.9198 | 0.1533 | 0.1278 | 0.068* | |
C14 | 0.7601 (14) | 0.1535 (8) | 0.0562 (7) | 0.055 (3) | |
H14 | 0.8251 | 0.1062 | 0.0181 | 0.066* | |
C15 | 0.6067 (14) | 0.1949 (9) | 0.0454 (7) | 0.055 (3) | |
H15 | 0.5691 | 0.1758 | −0.0001 | 0.065* | |
C16 | 0.5089 (12) | 0.2652 (8) | 0.1025 (6) | 0.043 (2) | |
H16 | 0.4064 | 0.2944 | 0.0946 | 0.052* | |
C2 | −0.1590 (13) | 0.7724 (9) | −0.0069 (7) | 0.053 (3) | |
C21 | 0.2960 (10) | 0.3246 (7) | 0.2968 (6) | 0.036 (2) | |
C22 | 0.2123 (13) | 0.2742 (8) | 0.2546 (7) | 0.051 (3) | |
H22 | 0.2339 | 0.2666 | 0.1986 | 0.061* | |
C23 | 0.0957 (14) | 0.2346 (10) | 0.2951 (9) | 0.066 (3) | |
H23 | 0.039 | 0.2022 | 0.266 | 0.079* | |
C24 | 0.0661 (15) | 0.2435 (10) | 0.3758 (9) | 0.068 (3) | |
H24 | −0.0096 | 0.216 | 0.4029 | 0.081* | |
C25 | 0.1484 (16) | 0.2938 (11) | 0.4184 (8) | 0.067 (3) | |
H25 | 0.1255 | 0.3018 | 0.4743 | 0.081* | |
C26 | 0.2633 (13) | 0.3319 (9) | 0.3793 (6) | 0.051 (3) | |
H26 | 0.32 | 0.3633 | 0.4092 | 0.061* | |
C31 | 0.3424 (10) | 0.4917 (7) | 0.1951 (5) | 0.0317 (19) | |
C32 | 0.1971 (9) | 0.5045 (7) | 0.1650 (5) | 0.0321 (19) | |
H32 | 0.1366 | 0.4578 | 0.1704 | 0.039* | |
C33 | 0.1607 (10) | 0.5986 (7) | 0.1262 (5) | 0.034 (2) | |
H33 | 0.073 | 0.6248 | 0.1008 | 0.041* | |
C34 | 0.2803 (10) | 0.6472 (7) | 0.1322 (5) | 0.0308 (19) | |
H34 | 0.2846 | 0.711 | 0.1116 | 0.037* | |
C35 | 0.3927 (10) | 0.5821 (6) | 0.1750 (5) | 0.0278 (17) | |
C36 | 0.5484 (10) | 0.5976 (7) | 0.1899 (6) | 0.035 (2) | |
H36 | 0.55 | 0.5984 | 0.2486 | 0.042* | |
C37 | 0.5713 (11) | 0.7014 (8) | 0.1597 (7) | 0.049 (3) | |
H37A | 0.6705 | 0.7077 | 0.1708 | 0.073* | |
H37B | 0.4911 | 0.7571 | 0.1869 | 0.073* | |
H37C | 0.5668 | 0.7043 | 0.1025 | 0.073* | |
C38 | 0.6793 (13) | 0.4901 (9) | 0.0679 (6) | 0.052 (3) | |
H38A | 0.5791 | 0.4922 | 0.0531 | 0.079* | |
H38B | 0.7502 | 0.4245 | 0.051 | 0.079* | |
H38C | 0.7161 | 0.5446 | 0.0419 | 0.079* | |
C39 | 0.8199 (11) | 0.4994 (9) | 0.1804 (7) | 0.055 (3) | |
H39A | 0.8941 | 0.4383 | 0.1567 | 0.082* | |
H39B | 0.8135 | 0.4973 | 0.2382 | 0.082* | |
H39C | 0.8516 | 0.5595 | 0.1624 | 0.082* | |
C41 | 0.0706 (10) | 0.7584 (7) | 0.3023 (6) | 0.037 (2) | |
C42 | 0.2004 (12) | 0.7087 (7) | 0.3423 (5) | 0.037 (2) | |
H42 | 0.283 | 0.7357 | 0.3496 | 0.045* | |
C43 | 0.1831 (13) | 0.6127 (8) | 0.3687 (6) | 0.049 (3) | |
H43 | 0.2529 | 0.5649 | 0.3956 | 0.058* | |
C44 | 0.0430 (12) | 0.6005 (8) | 0.3476 (6) | 0.048 (3) | |
H44 | 0.0032 | 0.5439 | 0.3587 | 0.057* | |
C45 | −0.0260 (12) | 0.6880 (7) | 0.3072 (6) | 0.043 (2) | |
H45 | −0.12 | 0.6993 | 0.2865 | 0.051* | |
C51 | −0.1164 (17) | 0.9604 (9) | 0.3425 (8) | 0.0704 (15) | |
C52 | −0.1513 (16) | 0.9208 (9) | 0.4165 (7) | 0.0704 (15) | |
H52 | −0.1017 | 0.8529 | 0.4271 | 0.084* | |
C53 | −0.2557 (17) | 0.9791 (9) | 0.4731 (8) | 0.0704 (15) | |
H53 | −0.2819 | 0.949 | 0.5212 | 0.084* | |
C54 | −0.3280 (16) | 1.0849 (9) | 0.4628 (8) | 0.0704 (15) | |
H54 | −0.3917 | 1.1272 | 0.5045 | 0.084* | |
C55 | −0.2977 (17) | 1.1206 (9) | 0.3875 (8) | 0.0704 (15) | |
H55 | −0.3493 | 1.1879 | 0.3761 | 0.084* | |
C56 | −0.1950 (16) | 1.0613 (9) | 0.3291 (8) | 0.0704 (15) | |
H56 | −0.177 | 1.089 | 0.2788 | 0.084* | |
C61 | 0.1842 (11) | 0.9311 (7) | 0.2468 (6) | 0.039 (2) | |
C62 | 0.2665 (14) | 0.9406 (9) | 0.3113 (7) | 0.055 (3) | |
H62 | 0.2317 | 0.9237 | 0.363 | 0.066* | |
C63 | 0.4000 (15) | 0.9752 (11) | 0.2983 (8) | 0.067 (3) | |
H63 | 0.4573 | 0.9772 | 0.3407 | 0.081* | |
C64 | 0.4462 (14) | 1.0058 (9) | 0.2247 (9) | 0.063 (3) | |
H64 | 0.5329 | 1.0315 | 0.2173 | 0.075* | |
C65 | 0.3676 (15) | 0.9995 (9) | 0.1604 (8) | 0.057 (3) | |
H65 | 0.4016 | 1.0197 | 0.1096 | 0.069* | |
C66 | 0.2362 (12) | 0.9625 (8) | 0.1719 (7) | 0.046 (2) | |
H66 | 0.1822 | 0.9589 | 0.1284 | 0.056* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au1 | 0.0326 (2) | 0.0326 (2) | 0.0419 (2) | −0.00665 (15) | −0.01257 (16) | −0.00029 (16) |
Au2 | 0.0431 (3) | 0.0333 (2) | 0.0414 (3) | −0.00277 (17) | −0.01233 (17) | −0.00221 (16) |
P1 | 0.0241 (11) | 0.0229 (11) | 0.0399 (13) | −0.0014 (8) | −0.0081 (9) | −0.0012 (9) |
P2 | 0.0398 (13) | 0.0252 (12) | 0.0384 (13) | −0.0005 (10) | −0.0092 (10) | −0.0035 (9) |
S1 | 0.0562 (17) | 0.0641 (18) | 0.0530 (16) | −0.0221 (14) | −0.0253 (13) | −0.0002 (14) |
S2 | 0.069 (2) | 0.0500 (17) | 0.0584 (18) | −0.0029 (14) | −0.0330 (15) | −0.0017 (13) |
N1 | 0.112 (11) | 0.066 (9) | 0.132 (12) | −0.011 (8) | −0.055 (9) | −0.018 (8) |
N2 | 0.096 (9) | 0.081 (9) | 0.074 (8) | −0.035 (7) | −0.017 (7) | −0.022 (7) |
N3 | 0.018 (4) | 0.040 (4) | 0.051 (5) | −0.001 (3) | −0.005 (3) | −0.008 (4) |
Fe | 0.0231 (6) | 0.0221 (6) | 0.0377 (7) | −0.0009 (5) | −0.0032 (5) | 0.0022 (5) |
C1 | 0.057 (7) | 0.072 (9) | 0.067 (8) | −0.024 (7) | −0.016 (6) | −0.021 (7) |
C11 | 0.032 (5) | 0.021 (4) | 0.047 (5) | −0.006 (3) | −0.005 (4) | 0.002 (4) |
C12 | 0.032 (5) | 0.043 (6) | 0.054 (6) | −0.004 (4) | −0.009 (4) | 0.003 (5) |
C13 | 0.038 (6) | 0.046 (6) | 0.069 (8) | 0.013 (5) | 0.004 (5) | −0.006 (6) |
C14 | 0.061 (7) | 0.030 (5) | 0.062 (7) | 0.000 (5) | 0.008 (6) | 0.001 (5) |
C15 | 0.069 (8) | 0.049 (6) | 0.050 (6) | −0.021 (6) | −0.010 (5) | −0.006 (5) |
C16 | 0.043 (6) | 0.038 (5) | 0.045 (6) | −0.005 (4) | −0.004 (4) | −0.005 (4) |
C2 | 0.052 (7) | 0.058 (7) | 0.053 (7) | −0.017 (5) | −0.022 (5) | −0.006 (6) |
C21 | 0.031 (5) | 0.024 (4) | 0.058 (6) | −0.011 (4) | −0.012 (4) | 0.008 (4) |
C22 | 0.053 (7) | 0.039 (6) | 0.063 (7) | −0.013 (5) | −0.015 (5) | 0.009 (5) |
C23 | 0.047 (7) | 0.054 (7) | 0.103 (11) | −0.021 (6) | −0.020 (7) | 0.004 (7) |
C24 | 0.054 (8) | 0.065 (8) | 0.084 (10) | −0.025 (6) | 0.009 (7) | 0.011 (7) |
C25 | 0.082 (9) | 0.077 (9) | 0.052 (7) | −0.039 (7) | −0.006 (6) | 0.001 (6) |
C26 | 0.061 (7) | 0.052 (7) | 0.047 (6) | −0.025 (5) | −0.013 (5) | 0.003 (5) |
C31 | 0.031 (5) | 0.028 (4) | 0.036 (5) | −0.007 (4) | −0.005 (4) | −0.007 (4) |
C32 | 0.019 (4) | 0.026 (4) | 0.050 (5) | 0.000 (3) | −0.011 (4) | −0.002 (4) |
C33 | 0.022 (4) | 0.038 (5) | 0.039 (5) | −0.002 (4) | −0.009 (4) | 0.004 (4) |
C34 | 0.027 (4) | 0.033 (5) | 0.029 (4) | −0.001 (4) | −0.007 (3) | 0.007 (4) |
C35 | 0.024 (4) | 0.026 (4) | 0.032 (4) | −0.005 (3) | 0.000 (3) | −0.001 (3) |
C36 | 0.030 (5) | 0.031 (5) | 0.040 (5) | −0.004 (4) | −0.004 (4) | −0.005 (4) |
C37 | 0.029 (5) | 0.038 (5) | 0.086 (8) | −0.020 (4) | −0.012 (5) | 0.010 (5) |
C38 | 0.041 (6) | 0.062 (7) | 0.048 (6) | −0.008 (5) | 0.003 (5) | −0.008 (5) |
C39 | 0.030 (5) | 0.061 (7) | 0.072 (8) | −0.008 (5) | −0.011 (5) | −0.001 (6) |
C41 | 0.031 (5) | 0.030 (5) | 0.044 (5) | 0.002 (4) | −0.006 (4) | −0.007 (4) |
C42 | 0.044 (6) | 0.030 (5) | 0.034 (5) | −0.003 (4) | −0.004 (4) | −0.002 (4) |
C43 | 0.057 (7) | 0.046 (6) | 0.035 (5) | 0.000 (5) | −0.005 (5) | 0.002 (4) |
C44 | 0.042 (6) | 0.037 (6) | 0.053 (6) | 0.001 (4) | 0.013 (5) | 0.003 (5) |
C45 | 0.037 (5) | 0.036 (5) | 0.050 (6) | −0.006 (4) | 0.004 (4) | 0.001 (4) |
C51 | 0.092 (4) | 0.037 (3) | 0.061 (3) | 0.010 (2) | 0.009 (3) | 0.003 (2) |
C52 | 0.092 (4) | 0.037 (3) | 0.061 (3) | 0.010 (2) | 0.009 (3) | 0.003 (2) |
C53 | 0.092 (4) | 0.037 (3) | 0.061 (3) | 0.010 (2) | 0.009 (3) | 0.003 (2) |
C54 | 0.092 (4) | 0.037 (3) | 0.061 (3) | 0.010 (2) | 0.009 (3) | 0.003 (2) |
C55 | 0.092 (4) | 0.037 (3) | 0.061 (3) | 0.010 (2) | 0.009 (3) | 0.003 (2) |
C56 | 0.092 (4) | 0.037 (3) | 0.061 (3) | 0.010 (2) | 0.009 (3) | 0.003 (2) |
C61 | 0.046 (6) | 0.022 (4) | 0.047 (6) | −0.005 (4) | −0.011 (4) | −0.005 (4) |
C62 | 0.069 (8) | 0.063 (7) | 0.042 (6) | −0.031 (6) | −0.012 (5) | 0.011 (5) |
C63 | 0.063 (8) | 0.070 (9) | 0.078 (9) | −0.026 (7) | −0.028 (7) | −0.010 (7) |
C64 | 0.049 (7) | 0.048 (7) | 0.093 (10) | −0.014 (5) | −0.010 (7) | −0.001 (6) |
C65 | 0.062 (8) | 0.050 (7) | 0.057 (7) | −0.012 (6) | −0.005 (6) | −0.003 (5) |
C66 | 0.046 (6) | 0.042 (6) | 0.053 (6) | −0.015 (5) | −0.008 (5) | 0.003 (5) |
Au1—P1 | 2.265 (2) | C31—C32 | 1.429 (12) |
Au1—S1 | 2.327 (3) | C32—C33 | 1.396 (12) |
Au2—P2 | 2.260 (3) | C32—H32 | 0.93 |
Au2—S2 | 2.313 (3) | C33—C34 | 1.412 (13) |
P1—C31 | 1.799 (9) | C33—H33 | 0.93 |
P1—C11 | 1.813 (9) | C34—C35 | 1.418 (12) |
P1—C21 | 1.831 (9) | C34—H34 | 0.93 |
P2—C41 | 1.769 (10) | C35—C36 | 1.522 (12) |
P2—C61 | 1.803 (10) | C36—C37 | 1.535 (13) |
P2—C51 | 1.816 (12) | C36—H36 | 0.98 |
S1—C1 | 1.678 (15) | C37—H37A | 0.96 |
S2—C2 | 1.673 (12) | C37—H37B | 0.96 |
N1—C1 | 1.158 (18) | C37—H37C | 0.96 |
N2—C2 | 1.133 (16) | C38—H38A | 0.96 |
N3—C39 | 1.463 (12) | C38—H38B | 0.96 |
N3—C38 | 1.468 (13) | C38—H38C | 0.96 |
N3—C36 | 1.482 (11) | C39—H39A | 0.96 |
Fe—C32 | 2.023 (9) | C39—H39B | 0.96 |
Fe—C45 | 2.025 (10) | C39—H39C | 0.96 |
Fe—C31 | 2.029 (9) | C41—C42 | 1.428 (13) |
Fe—C35 | 2.032 (8) | C41—C45 | 1.439 (14) |
Fe—C41 | 2.036 (9) | C42—C43 | 1.400 (14) |
Fe—C42 | 2.044 (9) | C42—H42 | 0.93 |
Fe—C43 | 2.053 (10) | C43—C44 | 1.402 (16) |
Fe—C34 | 2.056 (9) | C43—H43 | 0.93 |
Fe—C44 | 2.057 (10) | C44—C45 | 1.391 (14) |
Fe—C33 | 2.060 (9) | C44—H44 | 0.93 |
C11—C16 | 1.392 (14) | C45—H45 | 0.93 |
C11—C12 | 1.395 (13) | C51—C52 | 1.377 (16) |
C12—C13 | 1.402 (14) | C51—C56 | 1.383 (16) |
C12—H12 | 0.93 | C52—C53 | 1.337 (16) |
C13—C14 | 1.348 (17) | C52—H52 | 0.93 |
C13—H13 | 0.93 | C53—C54 | 1.416 (16) |
C14—C15 | 1.383 (16) | C53—H53 | 0.93 |
C14—H14 | 0.93 | C54—C55 | 1.366 (17) |
C15—C16 | 1.389 (15) | C54—H54 | 0.93 |
C15—H15 | 0.93 | C55—C56 | 1.354 (16) |
C16—H16 | 0.93 | C55—H55 | 0.93 |
C21—C26 | 1.369 (14) | C56—H56 | 0.93 |
C21—C22 | 1.386 (14) | C61—C66 | 1.385 (14) |
C22—C23 | 1.401 (16) | C61—C62 | 1.403 (14) |
C22—H22 | 0.93 | C62—C63 | 1.393 (16) |
C23—C24 | 1.339 (18) | C62—H62 | 0.93 |
C23—H23 | 0.93 | C63—C64 | 1.347 (18) |
C24—C25 | 1.380 (19) | C63—H63 | 0.93 |
C24—H24 | 0.93 | C64—C65 | 1.370 (17) |
C25—C26 | 1.369 (16) | C64—H64 | 0.93 |
C25—H25 | 0.93 | C65—C66 | 1.393 (16) |
C26—H26 | 0.93 | C65—H65 | 0.93 |
C31—C35 | 1.427 (12) | C66—H66 | 0.93 |
P1—Au1—S1 | 175.61 (9) | C33—C32—H32 | 125.5 |
P2—Au2—S2 | 176.86 (9) | C31—C32—H32 | 125.5 |
C31—P1—C11 | 105.6 (4) | Fe—C32—H32 | 125 |
C31—P1—C21 | 105.8 (4) | C32—C33—C34 | 108.1 (7) |
C11—P1—C21 | 107.1 (4) | C32—C33—Fe | 68.6 (5) |
C31—P1—Au1 | 112.7 (3) | C34—C33—Fe | 69.8 (5) |
C11—P1—Au1 | 114.4 (3) | C32—C33—H33 | 126 |
C21—P1—Au1 | 110.6 (3) | C34—C33—H33 | 126 |
C41—P2—C61 | 107.3 (4) | Fe—C33—H33 | 127.2 |
C41—P2—C51 | 103.6 (5) | C33—C34—C35 | 108.4 (8) |
C61—P2—C51 | 106.7 (6) | C33—C34—Fe | 70.1 (5) |
C41—P2—Au2 | 113.4 (3) | C35—C34—Fe | 68.8 (5) |
C61—P2—Au2 | 113.2 (3) | C33—C34—H34 | 125.8 |
C51—P2—Au2 | 112.0 (5) | C35—C34—H34 | 125.8 |
C1—S1—Au1 | 95.9 (4) | Fe—C34—H34 | 126.9 |
C2—S2—Au2 | 103.1 (4) | C34—C35—C31 | 107.7 (8) |
C39—N3—C38 | 110.7 (8) | C34—C35—C36 | 127.3 (8) |
C39—N3—C36 | 112.0 (8) | C31—C35—C36 | 124.6 (8) |
C38—N3—C36 | 114.2 (8) | C34—C35—Fe | 70.6 (5) |
C32—Fe—C45 | 117.3 (4) | C31—C35—Fe | 69.3 (5) |
C32—Fe—C31 | 41.3 (3) | C36—C35—Fe | 130.5 (6) |
C45—Fe—C31 | 150.1 (4) | N3—C36—C35 | 106.6 (7) |
C32—Fe—C35 | 68.9 (3) | N3—C36—C37 | 115.7 (8) |
C45—Fe—C35 | 167.9 (4) | C35—C36—C37 | 112.6 (8) |
C31—Fe—C35 | 41.1 (3) | N3—C36—H36 | 107.2 |
C32—Fe—C41 | 151.0 (3) | C35—C36—H36 | 107.2 |
C45—Fe—C41 | 41.5 (4) | C37—C36—H36 | 107.2 |
C31—Fe—C41 | 166.6 (4) | C36—C37—H37A | 109.5 |
C35—Fe—C41 | 128.3 (4) | C36—C37—H37B | 109.5 |
C32—Fe—C42 | 166.3 (4) | H37A—C37—H37B | 109.5 |
C45—Fe—C42 | 68.0 (4) | C36—C37—H37C | 109.5 |
C31—Fe—C42 | 128.0 (4) | H37A—C37—H37C | 109.5 |
C35—Fe—C42 | 108.5 (4) | H37B—C37—H37C | 109.5 |
C41—Fe—C42 | 41.0 (4) | N3—C38—H38A | 109.5 |
C32—Fe—C43 | 128.4 (4) | N3—C38—H38B | 109.5 |
C45—Fe—C43 | 67.3 (4) | H38A—C38—H38B | 109.5 |
C31—Fe—C43 | 107.5 (4) | N3—C38—H38C | 109.5 |
C35—Fe—C43 | 118.1 (4) | H38A—C38—H38C | 109.5 |
C41—Fe—C43 | 68.5 (4) | H38B—C38—H38C | 109.5 |
C42—Fe—C43 | 40.0 (4) | N3—C39—H39A | 109.5 |
C32—Fe—C34 | 67.7 (4) | N3—C39—H39B | 109.5 |
C45—Fe—C34 | 130.0 (4) | H39A—C39—H39B | 109.5 |
C31—Fe—C34 | 68.5 (4) | N3—C39—H39C | 109.5 |
C35—Fe—C34 | 40.6 (3) | H39A—C39—H39C | 109.5 |
C41—Fe—C34 | 108.7 (4) | H39B—C39—H39C | 109.5 |
C42—Fe—C34 | 119.6 (4) | C42—C41—C45 | 105.1 (8) |
C43—Fe—C34 | 152.2 (4) | C42—C41—P2 | 132.1 (7) |
C32—Fe—C44 | 108.0 (4) | C45—C41—P2 | 122.6 (7) |
C45—Fe—C44 | 39.8 (4) | C42—C41—Fe | 69.8 (5) |
C31—Fe—C44 | 117.0 (4) | C45—C41—Fe | 68.8 (5) |
C35—Fe—C44 | 150.8 (4) | P2—C41—Fe | 129.2 (5) |
C41—Fe—C44 | 68.7 (4) | C43—C42—C41 | 108.9 (9) |
C42—Fe—C44 | 67.4 (4) | C43—C42—Fe | 70.4 (6) |
C43—Fe—C44 | 39.9 (5) | C41—C42—Fe | 69.2 (5) |
C34—Fe—C44 | 167.1 (4) | C43—C42—H42 | 125.5 |
C32—Fe—C33 | 40.0 (4) | C41—C42—H42 | 125.5 |
C45—Fe—C33 | 109.2 (4) | Fe—C42—H42 | 126.5 |
C31—Fe—C33 | 68.4 (3) | C42—C43—C44 | 108.6 (9) |
C35—Fe—C33 | 68.2 (3) | C42—C43—Fe | 69.7 (6) |
C41—Fe—C33 | 118.5 (4) | C44—C43—Fe | 70.2 (6) |
C42—Fe—C33 | 152.7 (4) | C42—C43—H43 | 125.7 |
C43—Fe—C33 | 166.1 (4) | C44—C43—H43 | 125.7 |
C34—Fe—C33 | 40.1 (4) | Fe—C43—H43 | 126 |
C44—Fe—C33 | 129.0 (4) | C45—C44—C43 | 108.0 (10) |
N1—C1—S1 | 178.7 (13) | C45—C44—Fe | 68.8 (6) |
C16—C11—C12 | 118.9 (9) | C43—C44—Fe | 69.9 (6) |
C16—C11—P1 | 123.1 (7) | C45—C44—H44 | 126 |
C12—C11—P1 | 118.0 (7) | C43—C44—H44 | 126 |
C11—C12—C13 | 119.6 (10) | Fe—C44—H44 | 126.8 |
C11—C12—H12 | 120.2 | C44—C45—C41 | 109.4 (10) |
C13—C12—H12 | 120.2 | C44—C45—Fe | 71.3 (6) |
C14—C13—C12 | 120.7 (10) | C41—C45—Fe | 69.7 (5) |
C14—C13—H13 | 119.6 | C44—C45—H45 | 125.3 |
C12—C13—H13 | 119.6 | C41—C45—H45 | 125.3 |
C13—C14—C15 | 120.6 (10) | Fe—C45—H45 | 125.3 |
C13—C14—H14 | 119.7 | C52—C51—C56 | 117.5 (11) |
C15—C14—H14 | 119.7 | C52—C51—P2 | 122.5 (9) |
C14—C15—C16 | 119.9 (10) | C56—C51—P2 | 119.8 (10) |
C14—C15—H15 | 120.1 | C53—C52—C51 | 120.6 (11) |
C16—C15—H15 | 120.1 | C53—C52—H52 | 119.7 |
C15—C16—C11 | 120.3 (10) | C51—C52—H52 | 119.7 |
C15—C16—H16 | 119.9 | C52—C53—C54 | 122.5 (12) |
C11—C16—H16 | 119.9 | C52—C53—H53 | 118.7 |
N2—C2—S2 | 174.5 (12) | C54—C53—H53 | 118.7 |
C26—C21—C22 | 117.7 (9) | C55—C54—C53 | 115.4 (11) |
C26—C21—P1 | 118.4 (7) | C55—C54—H54 | 122.3 |
C22—C21—P1 | 123.9 (8) | C53—C54—H54 | 122.3 |
C21—C22—C23 | 120.8 (11) | C56—C55—C54 | 122.1 (11) |
C21—C22—H22 | 119.6 | C56—C55—H55 | 119 |
C23—C22—H22 | 119.6 | C54—C55—H55 | 119 |
C24—C23—C22 | 119.9 (12) | C55—C56—C51 | 121.4 (12) |
C24—C23—H23 | 120 | C55—C56—H56 | 119.3 |
C22—C23—H23 | 120 | C51—C56—H56 | 119.3 |
C23—C24—C25 | 119.7 (12) | C66—C61—C62 | 117.4 (9) |
C23—C24—H24 | 120.2 | C66—C61—P2 | 121.1 (7) |
C25—C24—H24 | 120.2 | C62—C61—P2 | 121.5 (8) |
C26—C25—C24 | 120.7 (12) | C63—C62—C61 | 120.5 (10) |
C26—C25—H25 | 119.7 | C63—C62—H62 | 119.7 |
C24—C25—H25 | 119.7 | C61—C62—H62 | 119.7 |
C25—C26—C21 | 121.1 (10) | C64—C63—C62 | 120.2 (11) |
C25—C26—H26 | 119.5 | C64—C63—H63 | 119.9 |
C21—C26—H26 | 119.5 | C62—C63—H63 | 119.9 |
C35—C31—C32 | 106.8 (8) | C63—C64—C65 | 121.1 (12) |
C35—C31—P1 | 125.8 (7) | C63—C64—H64 | 119.4 |
C32—C31—P1 | 127.4 (7) | C65—C64—H64 | 119.4 |
C35—C31—Fe | 69.5 (5) | C64—C65—C66 | 119.3 (12) |
C32—C31—Fe | 69.1 (5) | C64—C65—H65 | 120.4 |
P1—C31—Fe | 125.9 (5) | C66—C65—H65 | 120.4 |
C33—C32—C31 | 108.9 (8) | C61—C66—C65 | 121.4 (10) |
C33—C32—Fe | 71.4 (5) | C61—C66—H66 | 119.3 |
C31—C32—Fe | 69.6 (5) | C65—C66—H66 | 119.3 |
D—H···A | D—H | H···A | D···A | D—H···A |
C54—H54···N1i | 0.93 | 2.61 | 3.501 (18) | 160 |
Symmetry code: (i) −x, −y+2, −z+1. |
Complex | Au–P | Au–X | P–Au–X |
[(dppf)(AuCl)2]a | 2.226 (1) | 2.278 (1) | 177.56 (8) |
[(dppf-R)(AuCl)2]b | 2.237 (2) | 2.271 (3) | 175.4 (1) |
2.224 (2) | 2.278 (2) | 174.0 (1) | |
[(dppf-R)(AuSCN)2]c | 2.265 (2) | 2.327 (3) | 175.61 (9) |
2.260 (3) | 2.313 (3) | 176.86 (9) | |
[(dppf)(AuI)2]d | 2.248 (9) | 2.545 (3) | 177.7 (2) |
2.240 (8) | 2.561 (2) | 176.3 (2) | |
[(dppf-L)2(AuCl)3]e | 2.31 (2) | 2.52 (3) | 113 (2) |
2.28 (2) | 2.20 (2) | 177 (2) |
Notes: (a) Crespo et al. (2000); (b) Sam et al. (2005), R = -CH(CH3)N(CH3)2, dppf is 1,1'-bis(diphenylphosphino)ferrocene; (c) this work, R = -CH(CH3)N(CH3)2; (d) Canales et al. (1997), isolated as the CH2Cl2 solvate. (e) Togni et al. (1990), L = -CH(CH3)N(CH3)CH2CH2N(CH3)2, isolated as the Et2O solvate. |
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