

Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536810054115/ya2134sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536810054115/ya2134Isup2.hkl |
CCDC reference: 811150
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean
(C-C) = 0.008 Å
- R factor = 0.027
- wR factor = 0.058
- Data-to-parameter ratio = 16.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.16 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.47 Ratio PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 16 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors of C56 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C57 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 3
Alert level G PLAT128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
A solution of AuCl (0.1 mmol, 23.5 mg) in 1 ml of H2O and bis(diphenylphosphanyl)methane (0.2 mmol, 77 mg) in 1 ml of THF were mixed and sealed in a 4 ml glass vial and kept at 333 K for 2 days. Then the mixture was cooled down to room temperature and was allowed to stand. After 5 days, colorless crystals suitable for the X-ray diffraction experiment were collected.
All H atoms were placed geometrically (C-H 0.95 Å and 0.99 Å for aromatic and methylene H atoms respectively) and treated as riding with Uiso(H) = 1.2Ueq(C). There are four residual peaks higher than 1 eÅ-3, each one in the vicinity of each of the Au atom at the distances of 0.881-0.991 Å.
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
![]() | Fig. 1. The molecular structure of the title compound with displacement ellipsoids drawn at the 30% probability level; hydrogen atoms are omitted. |
[Au4(C25H21P2)Cl3(C25H22P2)]·2C4H8O | F(000) = 3400 |
Mr = 1806.15 | Dx = 2.088 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 9747 reflections |
a = 14.9822 (6) Å | θ = 2.3–28.3° |
b = 14.6274 (6) Å | µ = 10.47 mm−1 |
c = 27.1356 (10) Å | T = 100 K |
β = 104.981 (1)° | Block, colorless |
V = 5744.7 (4) Å3 | 0.22 × 0.20 × 0.18 mm |
Z = 4 |
Bruker SMART CCD area-detector diffractometer | 10683 independent reflections |
Radiation source: fine-focus sealed tube | 9041 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
phi and ω scans | θmax = 25.5°, θmin = 1.4° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −18→15 |
Tmin = 0.115, Tmax = 0.152 | k = −17→16 |
31460 measured reflections | l = −32→32 |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.058 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0278P)2] where P = (Fo2 + 2Fc2)/3 |
10683 reflections | (Δ/σ)max = 0.002 |
640 parameters | Δρmax = 1.32 e Å−3 |
0 restraints | Δρmin = −0.61 e Å−3 |
[Au4(C25H21P2)Cl3(C25H22P2)]·2C4H8O | V = 5744.7 (4) Å3 |
Mr = 1806.15 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 14.9822 (6) Å | µ = 10.47 mm−1 |
b = 14.6274 (6) Å | T = 100 K |
c = 27.1356 (10) Å | 0.22 × 0.20 × 0.18 mm |
β = 104.981 (1)° |
Bruker SMART CCD area-detector diffractometer | 10683 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | 9041 reflections with I > 2σ(I) |
Tmin = 0.115, Tmax = 0.152 | Rint = 0.034 |
31460 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 0 restraints |
wR(F2) = 0.058 | H-atom parameters constrained |
S = 0.99 | Δρmax = 1.32 e Å−3 |
10683 reflections | Δρmin = −0.61 e Å−3 |
640 parameters |
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. 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 > 2sigma(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 | 0.821477 (13) | 0.165214 (13) | 0.399909 (7) | 0.01754 (5) | |
Au2 | 0.729665 (13) | 0.371899 (13) | 0.398530 (7) | 0.01955 (5) | |
Au3 | 0.830843 (12) | 0.267477 (13) | 0.528113 (7) | 0.01567 (5) | |
Au4 | 0.821891 (13) | 0.276224 (13) | 0.648058 (8) | 0.01946 (5) | |
Cl1 | 0.92100 (8) | 0.18934 (9) | 0.34889 (5) | 0.0225 (3) | |
Cl2 | 0.80684 (10) | 0.44543 (10) | 0.34719 (5) | 0.0330 (3) | |
Cl4 | 0.70061 (9) | 0.17746 (9) | 0.63746 (5) | 0.0295 (3) | |
P1 | 0.73048 (9) | 0.12581 (9) | 0.45001 (5) | 0.0168 (3) | |
P2 | 0.64608 (9) | 0.31387 (9) | 0.44833 (5) | 0.0175 (3) | |
P3 | 0.97673 (9) | 0.31433 (9) | 0.56659 (5) | 0.0161 (3) | |
P4 | 0.93872 (9) | 0.37510 (9) | 0.66646 (5) | 0.0167 (3) | |
O1 | 0.4371 (3) | 0.2321 (3) | 0.54344 (19) | 0.0568 (13) | |
O2 | 0.4516 (4) | 0.4614 (3) | 0.26736 (19) | 0.0697 (16) | |
C1 | 0.6251 (3) | 0.0689 (3) | 0.41479 (18) | 0.0180 (11) | |
C2 | 0.5989 (4) | 0.0764 (4) | 0.3627 (2) | 0.0346 (15) | |
H2A | 0.6367 | 0.1085 | 0.3454 | 0.041* | |
C3 | 0.5162 (4) | 0.0368 (5) | 0.3354 (2) | 0.0451 (18) | |
H3A | 0.4968 | 0.0439 | 0.2994 | 0.054* | |
C4 | 0.4635 (4) | −0.0115 (4) | 0.3596 (2) | 0.0356 (15) | |
H4A | 0.4077 | −0.0390 | 0.3406 | 0.043* | |
C5 | 0.4906 (4) | −0.0209 (4) | 0.4121 (2) | 0.0335 (14) | |
H5A | 0.4541 | −0.0556 | 0.4291 | 0.040* | |
C6 | 0.5703 (4) | 0.0200 (4) | 0.4393 (2) | 0.0277 (13) | |
H6A | 0.5882 | 0.0147 | 0.4754 | 0.033* | |
C7 | 0.8515 (4) | −0.0167 (4) | 0.4873 (2) | 0.0282 (13) | |
H7A | 0.8688 | −0.0110 | 0.4562 | 0.034* | |
C8 | 0.8916 (4) | −0.0829 (4) | 0.5219 (2) | 0.0406 (16) | |
H8A | 0.9359 | −0.1231 | 0.5143 | 0.049* | |
C9 | 0.8682 (4) | −0.0914 (4) | 0.5676 (2) | 0.0323 (14) | |
H9A | 0.8961 | −0.1376 | 0.5912 | 0.039* | |
C10 | 0.8047 (4) | −0.0332 (4) | 0.5790 (2) | 0.0304 (13) | |
H10A | 0.7889 | −0.0390 | 0.6105 | 0.036* | |
C11 | 0.7632 (4) | 0.0346 (3) | 0.54457 (19) | 0.0228 (12) | |
H11A | 0.7199 | 0.0756 | 0.5527 | 0.027* | |
C12 | 0.7862 (3) | 0.0416 (3) | 0.49766 (18) | 0.0190 (11) | |
C13 | 0.7005 (3) | 0.2186 (3) | 0.48621 (18) | 0.0150 (10) | |
H13A | 0.6628 | 0.1967 | 0.5094 | 0.018* | |
C14 | 0.5300 (3) | 0.2836 (3) | 0.4117 (2) | 0.0230 (12) | |
C15 | 0.4999 (4) | 0.3097 (4) | 0.3611 (2) | 0.0353 (15) | |
H15A | 0.5399 | 0.3431 | 0.3456 | 0.042* | |
C16 | 0.4112 (4) | 0.2871 (5) | 0.3327 (3) | 0.0431 (17) | |
H16A | 0.3900 | 0.3058 | 0.2982 | 0.052* | |
C17 | 0.3556 (5) | 0.2382 (5) | 0.3550 (3) | 0.0507 (19) | |
H17A | 0.2950 | 0.2233 | 0.3355 | 0.061* | |
C18 | 0.3839 (4) | 0.2096 (4) | 0.4047 (3) | 0.0422 (17) | |
H18A | 0.3442 | 0.1736 | 0.4191 | 0.051* | |
C19 | 0.4719 (4) | 0.2338 (4) | 0.4341 (3) | 0.0336 (14) | |
H19A | 0.4917 | 0.2164 | 0.4689 | 0.040* | |
C20 | 0.6101 (3) | 0.4881 (3) | 0.4785 (2) | 0.0230 (12) | |
H20A | 0.6003 | 0.5029 | 0.4434 | 0.028* | |
C21 | 0.6037 (4) | 0.5561 (4) | 0.5126 (2) | 0.0282 (13) | |
H21A | 0.5884 | 0.6168 | 0.5009 | 0.034* | |
C22 | 0.6198 (3) | 0.5354 (4) | 0.5637 (2) | 0.0280 (13) | |
H22A | 0.6185 | 0.5824 | 0.5876 | 0.034* | |
C23 | 0.6378 (4) | 0.4463 (4) | 0.5800 (2) | 0.0303 (13) | |
H23A | 0.6470 | 0.4322 | 0.6152 | 0.036* | |
C24 | 0.6427 (3) | 0.3773 (4) | 0.5459 (2) | 0.0233 (12) | |
H24A | 0.6542 | 0.3160 | 0.5574 | 0.028* | |
C25 | 0.6304 (3) | 0.3988 (3) | 0.49429 (19) | 0.0190 (11) | |
C26 | 1.0386 (3) | 0.3562 (3) | 0.52206 (19) | 0.0171 (11) | |
C27 | 1.0185 (4) | 0.3184 (3) | 0.47360 (19) | 0.0215 (12) | |
H27A | 0.9694 | 0.2757 | 0.4638 | 0.026* | |
C28 | 1.0685 (4) | 0.3417 (4) | 0.4394 (2) | 0.0246 (12) | |
H28A | 1.0538 | 0.3152 | 0.4063 | 0.030* | |
C29 | 1.1403 (3) | 0.4036 (4) | 0.4535 (2) | 0.0236 (12) | |
H29A | 1.1767 | 0.4183 | 0.4306 | 0.028* | |
C30 | 1.1587 (4) | 0.4440 (4) | 0.5008 (2) | 0.0287 (13) | |
H30A | 1.2064 | 0.4883 | 0.5100 | 0.034* | |
C31 | 1.1088 (4) | 0.4211 (4) | 0.5351 (2) | 0.0271 (13) | |
H31A | 1.1222 | 0.4496 | 0.5677 | 0.033* | |
C32 | 1.1373 (4) | 0.2379 (4) | 0.6298 (2) | 0.0248 (12) | |
H32A | 1.1635 | 0.2973 | 0.6307 | 0.030* | |
C33 | 1.1891 (4) | 0.1670 (4) | 0.6566 (2) | 0.0280 (13) | |
H33A | 1.2502 | 0.1780 | 0.6765 | 0.034* | |
C34 | 1.1521 (4) | 0.0800 (4) | 0.6544 (2) | 0.0280 (13) | |
H34A | 1.1883 | 0.0315 | 0.6725 | 0.034* | |
C35 | 1.0638 (4) | 0.0636 (3) | 0.6265 (2) | 0.0266 (13) | |
H35A | 1.0388 | 0.0037 | 0.6251 | 0.032* | |
C36 | 1.0102 (4) | 0.1348 (3) | 0.59980 (19) | 0.0207 (11) | |
H36A | 0.9486 | 0.1235 | 0.5805 | 0.025* | |
C37 | 1.0472 (3) | 0.2224 (3) | 0.60168 (19) | 0.0186 (11) | |
C38 | 0.9833 (3) | 0.4068 (3) | 0.61248 (18) | 0.0163 (11) | |
H38A | 1.0485 | 0.4260 | 0.6253 | 0.020* | |
H38B | 0.9478 | 0.4598 | 0.5949 | 0.020* | |
C39 | 0.9083 (3) | 0.4827 (3) | 0.69037 (18) | 0.0182 (11) | |
C40 | 0.9591 (3) | 0.5624 (3) | 0.68955 (19) | 0.0211 (11) | |
H40A | 1.0100 | 0.5619 | 0.6747 | 0.025* | |
C41 | 0.9355 (4) | 0.6418 (4) | 0.7103 (2) | 0.0272 (13) | |
H41A | 0.9708 | 0.6956 | 0.7100 | 0.033* | |
C42 | 0.8605 (4) | 0.6442 (4) | 0.7316 (2) | 0.0303 (13) | |
H42A | 0.8445 | 0.6992 | 0.7458 | 0.036* | |
C43 | 0.8097 (4) | 0.5655 (4) | 0.7319 (2) | 0.0303 (13) | |
H43A | 0.7583 | 0.5666 | 0.7463 | 0.036* | |
C44 | 0.8327 (3) | 0.4859 (4) | 0.71156 (19) | 0.0228 (12) | |
H44A | 0.7970 | 0.4324 | 0.7119 | 0.027* | |
C45 | 1.0375 (4) | 0.2417 (4) | 0.73054 (19) | 0.0224 (12) | |
H45A | 0.9816 | 0.2076 | 0.7215 | 0.027* | |
C46 | 1.1162 (4) | 0.2022 (4) | 0.76134 (19) | 0.0245 (12) | |
H46A | 1.1150 | 0.1412 | 0.7732 | 0.029* | |
C47 | 1.1964 (4) | 0.2527 (3) | 0.77444 (19) | 0.0235 (12) | |
H47A | 1.2511 | 0.2258 | 0.7951 | 0.028* | |
C48 | 1.1986 (4) | 0.3414 (4) | 0.75816 (19) | 0.0243 (12) | |
H48A | 1.2544 | 0.3755 | 0.7680 | 0.029* | |
C49 | 1.1199 (3) | 0.3813 (4) | 0.72746 (19) | 0.0199 (11) | |
H49A | 1.1209 | 0.4429 | 0.7165 | 0.024* | |
C50 | 1.0389 (3) | 0.3297 (3) | 0.71279 (18) | 0.0162 (11) | |
C51 | 0.4491 (5) | 0.2656 (5) | 0.5949 (3) | 0.054 (2) | |
H51A | 0.4890 | 0.3206 | 0.6008 | 0.065* | |
H51B | 0.4780 | 0.2182 | 0.6200 | 0.065* | |
C52 | 0.3534 (5) | 0.2887 (6) | 0.5999 (3) | 0.070 (3) | |
H52A | 0.3490 | 0.2831 | 0.6356 | 0.084* | |
H52B | 0.3338 | 0.3508 | 0.5870 | 0.084* | |
C53 | 0.2995 (6) | 0.2156 (7) | 0.5663 (3) | 0.077 (3) | |
H53A | 0.3036 | 0.1570 | 0.5851 | 0.093* | |
H53B | 0.2337 | 0.2332 | 0.5540 | 0.093* | |
C54 | 0.3414 (5) | 0.2074 (5) | 0.5243 (3) | 0.058 (2) | |
H54A | 0.3360 | 0.1439 | 0.5112 | 0.069* | |
H54B | 0.3106 | 0.2488 | 0.4961 | 0.069* | |
C55 | 0.4912 (7) | 0.5337 (6) | 0.3012 (3) | 0.080 (3) | |
H55A | 0.5592 | 0.5338 | 0.3070 | 0.096* | |
H55B | 0.4766 | 0.5255 | 0.3344 | 0.096* | |
C56 | 0.4515 (8) | 0.6222 (6) | 0.2772 (3) | 0.112 (4) | |
H56A | 0.5011 | 0.6650 | 0.2744 | 0.134* | |
H56B | 0.4128 | 0.6515 | 0.2972 | 0.134* | |
C57 | 0.3939 (5) | 0.5940 (5) | 0.2249 (3) | 0.0517 (18) | |
H57A | 0.3272 | 0.5945 | 0.2235 | 0.062* | |
H57B | 0.4049 | 0.6350 | 0.1981 | 0.062* | |
C58 | 0.4262 (6) | 0.5006 (5) | 0.2190 (3) | 0.058 (2) | |
H58A | 0.3763 | 0.4645 | 0.1963 | 0.070* | |
H58B | 0.4797 | 0.5023 | 0.2040 | 0.070* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au1 | 0.01512 (11) | 0.01976 (11) | 0.01662 (11) | −0.00144 (8) | 0.00206 (8) | −0.00055 (8) |
Au2 | 0.02057 (11) | 0.01999 (11) | 0.01713 (11) | −0.00422 (8) | 0.00314 (9) | −0.00074 (8) |
Au3 | 0.01249 (10) | 0.01809 (10) | 0.01494 (11) | −0.00262 (7) | 0.00085 (8) | −0.00149 (7) |
Au4 | 0.01640 (11) | 0.02231 (11) | 0.01836 (11) | −0.00511 (8) | 0.00215 (9) | 0.00039 (8) |
Cl1 | 0.0166 (7) | 0.0295 (7) | 0.0206 (7) | 0.0000 (5) | 0.0035 (5) | 0.0009 (5) |
Cl2 | 0.0441 (9) | 0.0331 (8) | 0.0253 (8) | −0.0208 (6) | 0.0152 (7) | −0.0065 (6) |
Cl4 | 0.0243 (7) | 0.0347 (8) | 0.0292 (8) | −0.0154 (6) | 0.0063 (6) | −0.0004 (6) |
P1 | 0.0166 (7) | 0.0174 (7) | 0.0146 (7) | −0.0021 (5) | 0.0011 (6) | −0.0001 (5) |
P2 | 0.0131 (7) | 0.0199 (7) | 0.0173 (7) | −0.0013 (5) | −0.0003 (6) | −0.0008 (5) |
P3 | 0.0141 (7) | 0.0179 (7) | 0.0154 (7) | −0.0029 (5) | 0.0022 (6) | −0.0009 (5) |
P4 | 0.0156 (7) | 0.0178 (7) | 0.0151 (7) | −0.0014 (5) | 0.0010 (6) | 0.0008 (5) |
O1 | 0.053 (3) | 0.062 (3) | 0.057 (3) | 0.003 (2) | 0.017 (3) | −0.002 (3) |
O2 | 0.115 (5) | 0.045 (3) | 0.049 (3) | 0.027 (3) | 0.019 (3) | 0.008 (3) |
C1 | 0.020 (3) | 0.015 (3) | 0.016 (3) | −0.003 (2) | 0.000 (2) | −0.001 (2) |
C2 | 0.034 (4) | 0.048 (4) | 0.019 (3) | −0.026 (3) | 0.002 (3) | 0.006 (3) |
C3 | 0.049 (4) | 0.063 (5) | 0.017 (3) | −0.029 (3) | −0.003 (3) | 0.000 (3) |
C4 | 0.027 (3) | 0.046 (4) | 0.028 (3) | −0.023 (3) | −0.003 (3) | −0.001 (3) |
C5 | 0.033 (4) | 0.039 (4) | 0.029 (3) | −0.018 (3) | 0.010 (3) | 0.001 (3) |
C6 | 0.026 (3) | 0.037 (3) | 0.016 (3) | −0.011 (3) | −0.002 (2) | −0.001 (2) |
C7 | 0.034 (3) | 0.027 (3) | 0.022 (3) | 0.007 (2) | 0.004 (3) | −0.001 (2) |
C8 | 0.039 (4) | 0.037 (4) | 0.041 (4) | 0.019 (3) | 0.002 (3) | 0.002 (3) |
C9 | 0.033 (4) | 0.023 (3) | 0.032 (3) | 0.002 (3) | −0.008 (3) | 0.010 (3) |
C10 | 0.034 (3) | 0.027 (3) | 0.026 (3) | −0.005 (3) | 0.000 (3) | 0.005 (2) |
C11 | 0.021 (3) | 0.019 (3) | 0.023 (3) | −0.004 (2) | −0.002 (2) | 0.000 (2) |
C12 | 0.019 (3) | 0.020 (3) | 0.014 (3) | −0.004 (2) | −0.002 (2) | 0.001 (2) |
C13 | 0.008 (2) | 0.022 (3) | 0.013 (3) | −0.0027 (19) | 0.001 (2) | 0.000 (2) |
C14 | 0.017 (3) | 0.018 (3) | 0.031 (3) | 0.003 (2) | 0.000 (2) | −0.002 (2) |
C15 | 0.026 (3) | 0.048 (4) | 0.027 (3) | 0.006 (3) | 0.000 (3) | −0.010 (3) |
C16 | 0.023 (3) | 0.058 (5) | 0.041 (4) | 0.005 (3) | −0.005 (3) | −0.010 (3) |
C17 | 0.028 (4) | 0.042 (4) | 0.065 (5) | 0.003 (3) | −0.020 (4) | −0.010 (4) |
C18 | 0.027 (4) | 0.033 (4) | 0.062 (5) | −0.012 (3) | 0.002 (3) | 0.004 (3) |
C19 | 0.019 (3) | 0.025 (3) | 0.051 (4) | 0.000 (2) | 0.000 (3) | 0.000 (3) |
C20 | 0.017 (3) | 0.023 (3) | 0.029 (3) | 0.000 (2) | 0.007 (2) | 0.000 (2) |
C21 | 0.021 (3) | 0.024 (3) | 0.041 (4) | −0.002 (2) | 0.010 (3) | 0.000 (3) |
C22 | 0.014 (3) | 0.034 (3) | 0.034 (3) | −0.002 (2) | 0.003 (3) | −0.014 (3) |
C23 | 0.022 (3) | 0.045 (4) | 0.023 (3) | 0.007 (3) | 0.004 (3) | −0.006 (3) |
C24 | 0.017 (3) | 0.026 (3) | 0.026 (3) | 0.003 (2) | 0.004 (2) | −0.002 (2) |
C25 | 0.011 (3) | 0.022 (3) | 0.023 (3) | −0.006 (2) | 0.003 (2) | −0.003 (2) |
C26 | 0.017 (3) | 0.016 (3) | 0.017 (3) | 0.005 (2) | 0.002 (2) | 0.004 (2) |
C27 | 0.022 (3) | 0.020 (3) | 0.023 (3) | −0.004 (2) | 0.005 (2) | 0.003 (2) |
C28 | 0.029 (3) | 0.024 (3) | 0.020 (3) | −0.002 (2) | 0.005 (3) | −0.004 (2) |
C29 | 0.017 (3) | 0.030 (3) | 0.025 (3) | 0.005 (2) | 0.007 (2) | 0.006 (2) |
C30 | 0.022 (3) | 0.034 (3) | 0.030 (3) | −0.009 (2) | 0.006 (3) | −0.005 (3) |
C31 | 0.019 (3) | 0.040 (3) | 0.021 (3) | −0.011 (2) | 0.003 (2) | −0.007 (3) |
C32 | 0.020 (3) | 0.026 (3) | 0.026 (3) | −0.004 (2) | 0.001 (2) | −0.006 (2) |
C33 | 0.015 (3) | 0.034 (3) | 0.030 (3) | 0.005 (2) | −0.003 (3) | −0.003 (3) |
C34 | 0.032 (3) | 0.027 (3) | 0.025 (3) | 0.011 (2) | 0.008 (3) | 0.003 (2) |
C35 | 0.037 (4) | 0.014 (3) | 0.029 (3) | 0.000 (2) | 0.008 (3) | 0.002 (2) |
C36 | 0.024 (3) | 0.019 (3) | 0.019 (3) | −0.002 (2) | 0.005 (2) | −0.003 (2) |
C37 | 0.017 (3) | 0.020 (3) | 0.017 (3) | 0.002 (2) | 0.001 (2) | −0.002 (2) |
C38 | 0.015 (3) | 0.016 (3) | 0.018 (3) | −0.002 (2) | 0.004 (2) | −0.002 (2) |
C39 | 0.019 (3) | 0.019 (3) | 0.015 (3) | 0.004 (2) | 0.001 (2) | 0.002 (2) |
C40 | 0.021 (3) | 0.023 (3) | 0.019 (3) | 0.002 (2) | 0.004 (2) | 0.003 (2) |
C41 | 0.027 (3) | 0.019 (3) | 0.033 (3) | −0.004 (2) | 0.005 (3) | 0.001 (2) |
C42 | 0.030 (3) | 0.032 (3) | 0.029 (3) | 0.007 (3) | 0.008 (3) | −0.005 (3) |
C43 | 0.031 (3) | 0.036 (4) | 0.025 (3) | 0.006 (3) | 0.009 (3) | 0.000 (3) |
C44 | 0.018 (3) | 0.029 (3) | 0.021 (3) | −0.002 (2) | 0.005 (2) | −0.001 (2) |
C45 | 0.025 (3) | 0.026 (3) | 0.016 (3) | −0.004 (2) | 0.007 (2) | −0.001 (2) |
C46 | 0.030 (3) | 0.024 (3) | 0.017 (3) | 0.005 (2) | 0.001 (2) | 0.005 (2) |
C47 | 0.027 (3) | 0.024 (3) | 0.015 (3) | 0.005 (2) | −0.002 (2) | −0.001 (2) |
C48 | 0.020 (3) | 0.031 (3) | 0.018 (3) | −0.005 (2) | −0.001 (2) | −0.003 (2) |
C49 | 0.019 (3) | 0.022 (3) | 0.016 (3) | −0.005 (2) | 0.001 (2) | −0.001 (2) |
C50 | 0.017 (3) | 0.021 (3) | 0.009 (2) | −0.001 (2) | 0.000 (2) | 0.000 (2) |
C51 | 0.050 (5) | 0.074 (6) | 0.043 (4) | −0.007 (4) | 0.017 (4) | −0.006 (4) |
C52 | 0.051 (5) | 0.098 (7) | 0.073 (6) | −0.031 (4) | 0.037 (5) | −0.020 (5) |
C53 | 0.077 (6) | 0.105 (8) | 0.061 (6) | −0.028 (5) | 0.036 (5) | −0.040 (5) |
C54 | 0.048 (5) | 0.053 (5) | 0.075 (6) | −0.017 (4) | 0.022 (4) | −0.008 (4) |
C55 | 0.115 (8) | 0.070 (6) | 0.045 (5) | 0.032 (5) | 0.002 (5) | 0.000 (4) |
C56 | 0.195 (12) | 0.051 (6) | 0.057 (6) | 0.022 (6) | −0.025 (7) | 0.005 (4) |
C57 | 0.062 (5) | 0.041 (4) | 0.050 (5) | 0.001 (3) | 0.011 (4) | 0.009 (3) |
C58 | 0.078 (6) | 0.055 (5) | 0.043 (5) | 0.014 (4) | 0.019 (4) | 0.003 (4) |
Au1—P1 | 2.2356 (13) | C24—H24A | 0.9500 |
Au1—Cl1 | 2.3091 (12) | C26—C27 | 1.386 (7) |
Au1—Au2 | 3.3177 (3) | C26—C31 | 1.393 (7) |
Au2—P2 | 2.2338 (13) | C27—C28 | 1.378 (7) |
Au2—Cl2 | 2.2950 (13) | C27—H27A | 0.9500 |
Au3—C13 | 2.114 (5) | C28—C29 | 1.382 (7) |
Au3—P3 | 2.2710 (13) | C28—H28A | 0.9500 |
Au3—Au4 | 3.2945 (3) | C29—C30 | 1.375 (7) |
Au4—P4 | 2.2256 (13) | C29—H29A | 0.9500 |
Au4—Cl4 | 2.2806 (12) | C30—C31 | 1.377 (7) |
P1—C13 | 1.800 (5) | C30—H30A | 0.9500 |
P1—C1 | 1.822 (5) | C31—H31A | 0.9500 |
P1—C12 | 1.825 (5) | C32—C33 | 1.384 (7) |
P2—C13 | 1.797 (5) | C32—C37 | 1.387 (7) |
P2—C25 | 1.818 (5) | C32—H32A | 0.9500 |
P2—C14 | 1.820 (5) | C33—C34 | 1.382 (8) |
P3—C26 | 1.809 (5) | C33—H33A | 0.9500 |
P3—C37 | 1.819 (5) | C34—C35 | 1.366 (7) |
P3—C38 | 1.823 (5) | C34—H34A | 0.9500 |
P4—C39 | 1.805 (5) | C35—C36 | 1.397 (7) |
P4—C50 | 1.816 (5) | C35—H35A | 0.9500 |
P4—C38 | 1.820 (5) | C36—C37 | 1.393 (7) |
O1—C54 | 1.439 (8) | C36—H36A | 0.9500 |
O1—C51 | 1.447 (8) | C38—H38A | 0.9900 |
O2—C58 | 1.391 (8) | C38—H38B | 0.9900 |
O2—C55 | 1.424 (9) | C39—C40 | 1.396 (7) |
C1—C2 | 1.369 (7) | C39—C44 | 1.397 (7) |
C1—C6 | 1.381 (7) | C40—C41 | 1.376 (7) |
C2—C3 | 1.394 (8) | C40—H40A | 0.9500 |
C2—H2A | 0.9500 | C41—C42 | 1.391 (8) |
C3—C4 | 1.351 (8) | C41—H41A | 0.9500 |
C3—H3A | 0.9500 | C42—C43 | 1.381 (8) |
C4—C5 | 1.382 (8) | C42—H42A | 0.9500 |
C4—H4A | 0.9500 | C43—C44 | 1.371 (7) |
C5—C6 | 1.369 (7) | C43—H43A | 0.9500 |
C5—H5A | 0.9500 | C44—H44A | 0.9500 |
C6—H6A | 0.9500 | C45—C50 | 1.377 (7) |
C7—C8 | 1.374 (8) | C45—C46 | 1.384 (7) |
C7—C12 | 1.379 (7) | C45—H45A | 0.9500 |
C7—H7A | 0.9500 | C46—C47 | 1.377 (7) |
C8—C9 | 1.379 (8) | C46—H46A | 0.9500 |
C8—H8A | 0.9500 | C47—C48 | 1.373 (7) |
C9—C10 | 1.370 (8) | C47—H47A | 0.9500 |
C9—H9A | 0.9500 | C48—C49 | 1.385 (7) |
C10—C11 | 1.393 (7) | C48—H48A | 0.9500 |
C10—H10A | 0.9500 | C49—C50 | 1.396 (7) |
C11—C12 | 1.405 (7) | C49—H49A | 0.9500 |
C11—H11A | 0.9500 | C51—C52 | 1.513 (9) |
C13—H13A | 1.0000 | C51—H51A | 0.9900 |
C14—C15 | 1.385 (8) | C51—H51B | 0.9900 |
C14—C19 | 1.389 (7) | C52—C53 | 1.499 (10) |
C15—C16 | 1.392 (8) | C52—H52A | 0.9900 |
C15—H15A | 0.9500 | C52—H52B | 0.9900 |
C16—C17 | 1.352 (9) | C53—C54 | 1.443 (9) |
C16—H16A | 0.9500 | C53—H53A | 0.9900 |
C17—C18 | 1.371 (9) | C53—H53B | 0.9900 |
C17—H17A | 0.9500 | C54—H54A | 0.9900 |
C18—C19 | 1.399 (8) | C54—H54B | 0.9900 |
C18—H18A | 0.9500 | C55—C56 | 1.501 (11) |
C19—H19A | 0.9500 | C55—H55A | 0.9900 |
C20—C21 | 1.378 (7) | C55—H55B | 0.9900 |
C20—C25 | 1.384 (7) | C56—C57 | 1.514 (10) |
C20—H20A | 0.9500 | C56—H56A | 0.9900 |
C21—C22 | 1.378 (8) | C56—H56B | 0.9900 |
C21—H21A | 0.9500 | C57—C58 | 1.472 (9) |
C22—C23 | 1.380 (8) | C57—H57A | 0.9900 |
C22—H22A | 0.9500 | C57—H57B | 0.9900 |
C23—C24 | 1.385 (7) | C58—H58A | 0.9900 |
C23—H23A | 0.9500 | C58—H58B | 0.9900 |
C24—C25 | 1.401 (7) | ||
P1—Au1—Cl1 | 173.66 (5) | C26—C27—H27A | 119.4 |
P1—Au1—Au2 | 85.73 (3) | C27—C28—C29 | 119.6 (5) |
Cl1—Au1—Au2 | 100.61 (3) | C27—C28—H28A | 120.2 |
P2—Au2—Cl2 | 173.98 (5) | C29—C28—H28A | 120.2 |
P2—Au2—Au1 | 86.70 (3) | C30—C29—C28 | 119.6 (5) |
Cl2—Au2—Au1 | 99.29 (4) | C30—C29—H29A | 120.2 |
C13—Au3—P3 | 174.14 (13) | C28—C29—H29A | 120.2 |
C13—Au3—Au4 | 106.05 (13) | C29—C30—C31 | 121.0 (5) |
P3—Au3—Au4 | 79.29 (3) | C29—C30—H30A | 119.5 |
P4—Au4—Cl4 | 174.11 (5) | C31—C30—H30A | 119.5 |
P4—Au4—Au3 | 90.94 (3) | C30—C31—C26 | 120.0 (5) |
Cl4—Au4—Au3 | 94.90 (3) | C30—C31—H31A | 120.0 |
C13—P1—C1 | 109.0 (2) | C26—C31—H31A | 120.0 |
C13—P1—C12 | 104.8 (2) | C33—C32—C37 | 120.0 (5) |
C1—P1—C12 | 103.8 (2) | C33—C32—H32A | 120.0 |
C13—P1—Au1 | 114.53 (16) | C37—C32—H32A | 120.0 |
C1—P1—Au1 | 112.38 (16) | C34—C33—C32 | 120.3 (5) |
C12—P1—Au1 | 111.48 (17) | C34—C33—H33A | 119.9 |
C13—P2—C25 | 104.9 (2) | C32—C33—H33A | 119.9 |
C13—P2—C14 | 110.6 (2) | C35—C34—C33 | 120.3 (5) |
C25—P2—C14 | 105.4 (2) | C35—C34—H34A | 119.8 |
C13—P2—Au2 | 113.49 (16) | C33—C34—H34A | 119.8 |
C25—P2—Au2 | 110.31 (16) | C34—C35—C36 | 120.1 (5) |
C14—P2—Au2 | 111.61 (18) | C34—C35—H35A | 120.0 |
C26—P3—C37 | 105.7 (2) | C36—C35—H35A | 120.0 |
C26—P3—C38 | 105.0 (2) | C37—C36—C35 | 119.8 (5) |
C37—P3—C38 | 105.6 (2) | C37—C36—H36A | 120.1 |
C26—P3—Au3 | 113.18 (17) | C35—C36—H36A | 120.1 |
C37—P3—Au3 | 112.17 (17) | C32—C37—C36 | 119.5 (5) |
C38—P3—Au3 | 114.40 (16) | C32—C37—P3 | 121.2 (4) |
C39—P4—C50 | 108.1 (2) | C36—C37—P3 | 119.3 (4) |
C39—P4—C38 | 104.3 (2) | P4—C38—P3 | 113.3 (3) |
C50—P4—C38 | 104.0 (2) | P4—C38—H38A | 108.9 |
C39—P4—Au4 | 112.97 (17) | P3—C38—H38A | 108.9 |
C50—P4—Au4 | 112.27 (16) | P4—C38—H38B | 108.9 |
C38—P4—Au4 | 114.55 (16) | P3—C38—H38B | 108.9 |
C54—O1—C51 | 107.4 (5) | H38A—C38—H38B | 107.7 |
C58—O2—C55 | 105.6 (6) | C40—C39—C44 | 118.8 (5) |
C2—C1—C6 | 119.4 (5) | C40—C39—P4 | 122.2 (4) |
C2—C1—P1 | 118.9 (4) | C44—C39—P4 | 119.0 (4) |
C6—C1—P1 | 121.7 (4) | C41—C40—C39 | 119.9 (5) |
C1—C2—C3 | 119.6 (5) | C41—C40—H40A | 120.0 |
C1—C2—H2A | 120.2 | C39—C40—H40A | 120.0 |
C3—C2—H2A | 120.2 | C40—C41—C42 | 120.9 (5) |
C4—C3—C2 | 120.6 (6) | C40—C41—H41A | 119.6 |
C4—C3—H3A | 119.7 | C42—C41—H41A | 119.6 |
C2—C3—H3A | 119.7 | C43—C42—C41 | 119.1 (5) |
C3—C4—C5 | 120.0 (5) | C43—C42—H42A | 120.4 |
C3—C4—H4A | 120.0 | C41—C42—H42A | 120.4 |
C5—C4—H4A | 120.0 | C44—C43—C42 | 120.6 (5) |
C6—C5—C4 | 119.7 (5) | C44—C43—H43A | 119.7 |
C6—C5—H5A | 120.1 | C42—C43—H43A | 119.7 |
C4—C5—H5A | 120.1 | C43—C44—C39 | 120.7 (5) |
C5—C6—C1 | 120.7 (5) | C43—C44—H44A | 119.7 |
C5—C6—H6A | 119.7 | C39—C44—H44A | 119.7 |
C1—C6—H6A | 119.7 | C50—C45—C46 | 120.9 (5) |
C8—C7—C12 | 120.3 (5) | C50—C45—H45A | 119.5 |
C8—C7—H7A | 119.9 | C46—C45—H45A | 119.5 |
C12—C7—H7A | 119.9 | C47—C46—C45 | 118.9 (5) |
C7—C8—C9 | 120.7 (6) | C47—C46—H46A | 120.6 |
C7—C8—H8A | 119.7 | C45—C46—H46A | 120.6 |
C9—C8—H8A | 119.7 | C48—C47—C46 | 121.0 (5) |
C10—C9—C8 | 119.9 (5) | C48—C47—H47A | 119.5 |
C10—C9—H9A | 120.1 | C46—C47—H47A | 119.5 |
C8—C9—H9A | 120.1 | C47—C48—C49 | 120.3 (5) |
C9—C10—C11 | 120.5 (5) | C47—C48—H48A | 119.9 |
C9—C10—H10A | 119.7 | C49—C48—H48A | 119.9 |
C11—C10—H10A | 119.7 | C48—C49—C50 | 119.1 (5) |
C10—C11—C12 | 119.1 (5) | C48—C49—H49A | 120.4 |
C10—C11—H11A | 120.4 | C50—C49—H49A | 120.4 |
C12—C11—H11A | 120.4 | C45—C50—C49 | 119.7 (5) |
C7—C12—C11 | 119.5 (5) | C45—C50—P4 | 120.0 (4) |
C7—C12—P1 | 119.4 (4) | C49—C50—P4 | 120.1 (4) |
C11—C12—P1 | 121.1 (4) | O1—C51—C52 | 106.1 (6) |
P2—C13—P1 | 114.4 (3) | O1—C51—H51A | 110.5 |
P2—C13—Au3 | 105.4 (2) | C52—C51—H51A | 110.5 |
P1—C13—Au3 | 102.8 (2) | O1—C51—H51B | 110.5 |
P2—C13—H13A | 111.3 | C52—C51—H51B | 110.5 |
P1—C13—H13A | 111.3 | H51A—C51—H51B | 108.7 |
Au3—C13—H13A | 111.3 | C53—C52—C51 | 99.2 (7) |
C15—C14—C19 | 119.8 (5) | C53—C52—H52A | 111.9 |
C15—C14—P2 | 119.7 (4) | C51—C52—H52A | 111.9 |
C19—C14—P2 | 120.5 (4) | C53—C52—H52B | 111.9 |
C14—C15—C16 | 120.2 (6) | C51—C52—H52B | 111.9 |
C14—C15—H15A | 119.9 | H52A—C52—H52B | 109.6 |
C16—C15—H15A | 119.9 | C54—C53—C52 | 105.3 (6) |
C17—C16—C15 | 119.3 (7) | C54—C53—H53A | 110.7 |
C17—C16—H16A | 120.3 | C52—C53—H53A | 110.7 |
C15—C16—H16A | 120.3 | C54—C53—H53B | 110.7 |
C16—C17—C18 | 122.1 (6) | C52—C53—H53B | 110.7 |
C16—C17—H17A | 119.0 | H53A—C53—H53B | 108.8 |
C18—C17—H17A | 119.0 | O1—C54—C53 | 106.8 (6) |
C17—C18—C19 | 119.3 (6) | O1—C54—H54A | 110.4 |
C17—C18—H18A | 120.3 | C53—C54—H54A | 110.4 |
C19—C18—H18A | 120.3 | O1—C54—H54B | 110.4 |
C14—C19—C18 | 119.3 (6) | C53—C54—H54B | 110.4 |
C14—C19—H19A | 120.3 | H54A—C54—H54B | 108.6 |
C18—C19—H19A | 120.3 | O2—C55—C56 | 108.0 (7) |
C21—C20—C25 | 121.5 (5) | O2—C55—H55A | 110.1 |
C21—C20—H20A | 119.3 | C56—C55—H55A | 110.1 |
C25—C20—H20A | 119.3 | O2—C55—H55B | 110.1 |
C20—C21—C22 | 119.4 (5) | C56—C55—H55B | 110.1 |
C20—C21—H21A | 120.3 | H55A—C55—H55B | 108.4 |
C22—C21—H21A | 120.3 | C55—C56—C57 | 103.7 (7) |
C21—C22—C23 | 120.0 (5) | C55—C56—H56A | 111.0 |
C21—C22—H22A | 120.0 | C57—C56—H56A | 111.0 |
C23—C22—H22A | 120.0 | C55—C56—H56B | 111.0 |
C22—C23—C24 | 120.8 (5) | C57—C56—H56B | 111.0 |
C22—C23—H23A | 119.6 | H56A—C56—H56B | 109.0 |
C24—C23—H23A | 119.6 | C58—C57—C56 | 103.3 (6) |
C23—C24—C25 | 119.2 (5) | C58—C57—H57A | 111.1 |
C23—C24—H24A | 120.4 | C56—C57—H57A | 111.1 |
C25—C24—H24A | 120.4 | C58—C57—H57B | 111.1 |
C20—C25—C24 | 118.9 (5) | C56—C57—H57B | 111.1 |
C20—C25—P2 | 119.3 (4) | H57A—C57—H57B | 109.1 |
C24—C25—P2 | 121.7 (4) | O2—C58—C57 | 107.3 (6) |
C27—C26—C31 | 118.6 (5) | O2—C58—H58A | 110.3 |
C27—C26—P3 | 118.4 (4) | C57—C58—H58A | 110.3 |
C31—C26—P3 | 123.0 (4) | O2—C58—H58B | 110.3 |
C28—C27—C26 | 121.2 (5) | C57—C58—H58B | 110.3 |
C28—C27—H27A | 119.4 | H58A—C58—H58B | 108.5 |
P1—Au1—Au2—P2 | −0.37 (5) | C21—C20—C25—P2 | −175.6 (4) |
Cl1—Au1—Au2—P2 | 179.53 (5) | C23—C24—C25—C20 | −2.6 (7) |
P1—Au1—Au2—Cl2 | −179.83 (5) | C23—C24—C25—P2 | 174.4 (4) |
Cl1—Au1—Au2—Cl2 | 0.08 (5) | C13—P2—C25—C20 | 165.0 (4) |
C13—Au3—Au4—P4 | −159.40 (14) | C14—P2—C25—C20 | −78.2 (4) |
P3—Au3—Au4—P4 | 23.07 (5) | Au2—P2—C25—C20 | 42.5 (4) |
C13—Au3—Au4—Cl4 | 19.84 (14) | C13—P2—C25—C24 | −11.9 (5) |
P3—Au3—Au4—Cl4 | −157.70 (5) | C14—P2—C25—C24 | 104.9 (4) |
Au2—Au1—P1—C13 | −26.52 (17) | Au2—P2—C25—C24 | −134.5 (4) |
Au2—Au1—P1—C1 | 98.65 (17) | C37—P3—C26—C27 | 91.9 (4) |
Au2—Au1—P1—C12 | −145.32 (17) | C38—P3—C26—C27 | −156.7 (4) |
Au1—Au2—P2—C13 | 27.05 (17) | Au3—P3—C26—C27 | −31.3 (4) |
Au1—Au2—P2—C25 | 144.44 (18) | C37—P3—C26—C31 | −84.7 (5) |
Au1—Au2—P2—C14 | −98.71 (18) | C38—P3—C26—C31 | 26.7 (5) |
Au4—Au3—P3—C26 | −166.56 (17) | Au3—P3—C26—C31 | 152.1 (4) |
Au4—Au3—P3—C37 | 73.93 (17) | C31—C26—C27—C28 | 2.3 (8) |
Au4—Au3—P3—C38 | −46.32 (17) | P3—C26—C27—C28 | −174.5 (4) |
Au3—Au4—P4—C39 | 120.06 (17) | C26—C27—C28—C29 | 0.1 (8) |
Au3—Au4—P4—C50 | −117.43 (17) | C27—C28—C29—C30 | −2.5 (8) |
Au3—Au4—P4—C38 | 0.83 (18) | C28—C29—C30—C31 | 2.4 (8) |
C13—P1—C1—C2 | 111.2 (5) | C29—C30—C31—C26 | 0.1 (9) |
C12—P1—C1—C2 | −137.5 (5) | C27—C26—C31—C30 | −2.4 (8) |
Au1—P1—C1—C2 | −17.0 (5) | P3—C26—C31—C30 | 174.2 (4) |
C13—P1—C1—C6 | −67.5 (5) | C37—C32—C33—C34 | 1.5 (8) |
C12—P1—C1—C6 | 43.8 (5) | C32—C33—C34—C35 | −0.8 (8) |
Au1—P1—C1—C6 | 164.4 (4) | C33—C34—C35—C36 | −0.1 (8) |
C6—C1—C2—C3 | 1.6 (9) | C34—C35—C36—C37 | 0.3 (8) |
P1—C1—C2—C3 | −177.0 (5) | C33—C32—C37—C36 | −1.2 (8) |
C1—C2—C3—C4 | −2.3 (11) | C33—C32—C37—P3 | 179.3 (4) |
C2—C3—C4—C5 | 1.0 (11) | C35—C36—C37—C32 | 0.3 (7) |
C3—C4—C5—C6 | 0.9 (10) | C35—C36—C37—P3 | 179.8 (4) |
C4—C5—C6—C1 | −1.5 (9) | C26—P3—C37—C32 | 59.2 (5) |
C2—C1—C6—C5 | 0.2 (9) | C38—P3—C37—C32 | −51.8 (5) |
P1—C1—C6—C5 | 178.9 (5) | Au3—P3—C37—C32 | −177.0 (4) |
C12—C7—C8—C9 | −0.8 (9) | C26—P3—C37—C36 | −120.2 (4) |
C7—C8—C9—C10 | −0.4 (9) | C38—P3—C37—C36 | 128.8 (4) |
C8—C9—C10—C11 | 0.2 (9) | Au3—P3—C37—C36 | 3.5 (5) |
C9—C10—C11—C12 | 1.0 (8) | C39—P4—C38—P3 | −157.2 (3) |
C8—C7—C12—C11 | 2.1 (8) | C50—P4—C38—P3 | 89.7 (3) |
C8—C7—C12—P1 | −177.5 (5) | Au4—P4—C38—P3 | −33.2 (3) |
C10—C11—C12—C7 | −2.2 (7) | C26—P3—C38—P4 | −172.3 (3) |
C10—C11—C12—P1 | 177.4 (4) | C37—P3—C38—P4 | −60.8 (3) |
C13—P1—C12—C7 | −151.7 (4) | Au3—P3—C38—P4 | 63.0 (3) |
C1—P1—C12—C7 | 93.9 (4) | C50—P4—C39—C40 | 75.2 (5) |
Au1—P1—C12—C7 | −27.3 (5) | C38—P4—C39—C40 | −34.9 (5) |
C13—P1—C12—C11 | 28.7 (5) | Au4—P4—C39—C40 | −159.9 (4) |
C1—P1—C12—C11 | −85.7 (4) | C50—P4—C39—C44 | −103.2 (4) |
Au1—P1—C12—C11 | 153.1 (4) | C38—P4—C39—C44 | 146.6 (4) |
C25—P2—C13—P1 | −176.5 (2) | Au4—P4—C39—C44 | 21.6 (5) |
C14—P2—C13—P1 | 70.3 (3) | C44—C39—C40—C41 | 1.3 (8) |
Au2—P2—C13—P1 | −56.1 (3) | P4—C39—C40—C41 | −177.1 (4) |
C25—P2—C13—Au3 | −64.4 (3) | C39—C40—C41—C42 | −0.9 (8) |
C14—P2—C13—Au3 | −177.6 (2) | C40—C41—C42—C43 | 0.1 (9) |
Au2—P2—C13—Au3 | 56.1 (2) | C41—C42—C43—C44 | 0.1 (9) |
C1—P1—C13—P2 | −70.8 (3) | C42—C43—C44—C39 | 0.3 (8) |
C12—P1—C13—P2 | 178.6 (2) | C40—C39—C44—C43 | −1.0 (8) |
Au1—P1—C13—P2 | 56.1 (3) | P4—C39—C44—C43 | 177.4 (4) |
C1—P1—C13—Au3 | 175.6 (2) | C50—C45—C46—C47 | 0.5 (8) |
C12—P1—C13—Au3 | 64.9 (3) | C45—C46—C47—C48 | 1.1 (8) |
Au1—P1—C13—Au3 | −57.5 (2) | C46—C47—C48—C49 | −0.9 (8) |
Au4—Au3—C13—P2 | 111.11 (19) | C47—C48—C49—C50 | −0.9 (8) |
Au4—Au3—C13—P1 | −128.78 (17) | C46—C45—C50—C49 | −2.3 (7) |
C13—P2—C14—C15 | −136.6 (4) | C46—C45—C50—P4 | 172.7 (4) |
C25—P2—C14—C15 | 110.6 (5) | C48—C49—C50—C45 | 2.5 (7) |
Au2—P2—C14—C15 | −9.2 (5) | C48—C49—C50—P4 | −172.5 (4) |
C13—P2—C14—C19 | 42.7 (5) | C39—P4—C50—C45 | 128.0 (4) |
C25—P2—C14—C19 | −70.1 (5) | C38—P4—C50—C45 | −121.6 (4) |
Au2—P2—C14—C19 | 170.1 (4) | Au4—P4—C50—C45 | 2.7 (4) |
C19—C14—C15—C16 | 0.8 (8) | C39—P4—C50—C49 | −57.1 (4) |
P2—C14—C15—C16 | −179.9 (4) | C38—P4—C50—C49 | 53.3 (4) |
C14—C15—C16—C17 | −1.1 (9) | Au4—P4—C50—C49 | 177.7 (3) |
C15—C16—C17—C18 | −0.4 (10) | C54—O1—C51—C52 | −17.8 (8) |
C16—C17—C18—C19 | 2.1 (10) | O1—C51—C52—C53 | 33.9 (8) |
C15—C14—C19—C18 | 0.9 (8) | C51—C52—C53—C54 | −38.2 (10) |
P2—C14—C19—C18 | −178.4 (4) | C51—O1—C54—C53 | −6.9 (8) |
C17—C18—C19—C14 | −2.3 (9) | C52—C53—C54—O1 | 29.2 (10) |
C25—C20—C21—C22 | 1.4 (8) | C58—O2—C55—C56 | 25.4 (10) |
C20—C21—C22—C23 | −3.0 (8) | O2—C55—C56—C57 | −5.4 (11) |
C21—C22—C23—C24 | 1.9 (8) | C55—C56—C57—C58 | −15.1 (10) |
C22—C23—C24—C25 | 0.9 (8) | C55—O2—C58—C57 | −35.9 (8) |
C21—C20—C25—C24 | 1.4 (7) | C56—C57—C58—O2 | 31.8 (9) |
Experimental details
Crystal data | |
Chemical formula | [Au4(C25H21P2)Cl3(C25H22P2)]·2C4H8O |
Mr | 1806.15 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 100 |
a, b, c (Å) | 14.9822 (6), 14.6274 (6), 27.1356 (10) |
β (°) | 104.981 (1) |
V (Å3) | 5744.7 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 10.47 |
Crystal size (mm) | 0.22 × 0.20 × 0.18 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 1998) |
Tmin, Tmax | 0.115, 0.152 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 31460, 10683, 9041 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.058, 0.99 |
No. of reflections | 10683 |
No. of parameters | 640 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.32, −0.61 |
Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
The crystal structures of Au compounds with the bis(diphenylphosphanyl)methane ligand have been widely studied (see, for instance, Bruce et al., 2006; Feng et al., 1997; Sevillano et al., 2007). Herein, we report the bis(tetrahydrofurane) solvate of a new tetranuclear complex with this ligand and a rather peculiar non-symmetrical structure.
The molecule of the title compound, (Fig. 1) features two chemically different fragments derived from bis(diphenylphosphanyl)methane, one of which represents neutral molecule coordinated to two gold atoms through each of its P atoms [Au3-P3 2.2710 (13), Au4-P4 2.2256 (13) Å]. These gold atoms are bonded to each other [Au3-Au4 3.2945 (3) Å] thus closing the Au2P2C-ring. The Au4 atom also has a terminal chloro ligand [Au4-Cl4 2.2806 (12) Å], whereas the Au3 atom is bonded to the C13 atom belonging to the bis(diphenylphosphanyl)methyl group [Au3-C13 2.114 (5) Å], which in its turn has each of its phosphorus atoms P1 and P2 bonded to gold atoms of the Cl1-Au1-Au2-Cl2 fragment [Au1-P1 2.2356 (13) Å, Au2-P2 2.2338 (13) Å, Au1-Au2 3.3177 (3) Å, Au1-Cl1 2.3091 (12) Å, Au2-Cl2 2.2950 (13) Å], thus closing the second five-membered ring. Both five-memebered Au2P2C rings have envelope conformations, however the conformation of symmetrically substituted ring with Au1 and Au2 atoms has a mirror symmetry [displacement of the C13 atom from the almost exactly planar Au2P2 group being 0.740 (5) Å], whereas the second five-membered ring is not symmetrical with one of the phosphorus atoms (P3) in the flap position, its displacement from the plane of the rest of the atoms in this ring being 0.889 (1) Å.