Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536811000109/pb2050sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536811000109/pb2050Isup2.hkl |
CCDC reference: 688664
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.007 Å
- R factor = 0.026
- wR factor = 0.052
- Data-to-parameter ratio = Infin
checkCIF/PLATON results
No syntax errors found
Alert level A TYPE078_ALERT_1_A _refine_ls_number_parameters is not of type numb.
Alert level B PLAT923_ALERT_1_B S values in the CIF and FCF Differ by ....... 0.03 PLAT928_ALERT_1_B Reported and Calculated S value Differ by . 1.00
Alert level C PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 4 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors of O1 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors of C31 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C32 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C34 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 3
1 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Tetrahydrothiophenegold(I) chloride [(THT)AuCl] was suspended in THF. 0.5 equivalents of the ligand bis(diphenylphosphino)-1,2-diethylhydrazine dissolved in dichloromethane (DCM) was added to the stirred suspension. The suspension turned yellow and became clear and after a short time micro crystals started to form. Crystals of the molecule was obtained by halting stirring as soon as the reaction turned clear, crystals big enough for single-crystal X-Ray analysis formed overnight.
The H atoms were positioned geometrically and allowed to ride on their respective parent atoms, with C—H = 0.93 (Ar—H) or 0.96 (CH3) Å, and with Ueq = 1.2 (Ar—H) or 1.5 (CH3) Ueq(C).
Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) and Mercury (Macrae et al., 2008); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Au2Cl2(C28H30N2P2)]·2C4H8O | F(000) = 2056 |
Mr = 1065.52 | Dx = 1.837 Mg m−3 |
Orthorhombic, Pccn | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ab 2ac | Cell parameters from 8545 reflections |
a = 12.3275 (18) Å | θ = 6.1–55.9° |
b = 17.200 (3) Å | µ = 7.86 mm−1 |
c = 18.173 (3) Å | T = 173 K |
V = 3853.4 (10) Å3 | Prismic, colourless |
Z = 4 | 0.48 × 0.23 × 0.14 mm |
Bruker SMART CCD area-detector diffractometer | 4199 independent reflections |
Radiation source: fine-focus sealed tube | 3256 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
ϕ and ω scans | θmax = 27.0°, θmin = 2.0° |
Absorption correction: integration (SADABS; Bruker, 1999) | h = −11→15 |
Tmin = 0.116, Tmax = 0.406 | k = −21→21 |
23024 measured reflections | l = −22→23 |
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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0196P)2 + 3.5032P] where P = (Fo2 + 2Fc2)/3 |
4199 reflections | (Δ/σ)max = 0.002 |
209 parameters | Δρmax = 0.52 e Å−3 |
0 restraints | Δρmin = −1.22 e Å−3 |
[Au2Cl2(C28H30N2P2)]·2C4H8O | V = 3853.4 (10) Å3 |
Mr = 1065.52 | Z = 4 |
Orthorhombic, Pccn | Mo Kα radiation |
a = 12.3275 (18) Å | µ = 7.86 mm−1 |
b = 17.200 (3) Å | T = 173 K |
c = 18.173 (3) Å | 0.48 × 0.23 × 0.14 mm |
Bruker SMART CCD area-detector diffractometer | 4199 independent reflections |
Absorption correction: integration (SADABS; Bruker, 1999) | 3256 reflections with I > 2σ(I) |
Tmin = 0.116, Tmax = 0.406 | Rint = 0.045 |
23024 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 0 restraints |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.52 e Å−3 |
4199 reflections | Δρmin = −1.22 e Å−3 |
209 parameters |
Experimental. Reaction: bis(diphenylphosphino)-1,2-diethylhydrazine: 155 mg (0.34 mmol), (THT)AuCl: 200 mg (0.68 mmol), tetrahydrofuran: 2 ml, dichloromethane: 5 ml, Yield: 86%. Colourless to grey crystals. 1H NMR: (d-DMSO, 300 MHz) δH 7.90 (dq, Arom, J (1H-31P) = 28.9, J (1H-1H) = 7.1 Hz), 7.71 (d, Arom, J = 7.0 Hz), 7.60 (d, Arom, J = 7.1 Hz), 7.55 (d, Arom, J (1H-1H) = 7.0 Hz), 3.33 (bs, CH2CH3), 0.43 (t, CH2CH3, 3J (1H-1H) = 6.6 Hz). 13C NMR:(d-DMSO, 75 MHz) δC 132.3 (bs, Arom), 130.6 (m, Arom), 129.0 (s, Arom), 128.0 (bs, Arom), 43.6 (bs, CH2CH3), 14.1 (d, CH2CH3, 3J (13C-31P) = 16.1 Hz). 31P NMR:(d-DMSO, 121 MHz) δP 87.7. MS: 920 (2%, M), 885 (14%, M - Cl). EA: Calc: (Au2Cl2P2N2C28H30) C 36.50%, H 3.28%, N 3.04%, Found: C 35.42%, H 3.44%, N 2.64%. MP: 202 - 204 °C. |
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 | ||
Au | 0.816153 (12) | 0.172310 (9) | 1.064560 (8) | 0.02482 (5) | |
Cl | 0.73414 (9) | 0.12548 (7) | 1.16939 (5) | 0.0353 (3) | |
N | 0.8044 (2) | 0.26317 (18) | 0.90903 (17) | 0.0226 (7) | |
P | 0.89483 (8) | 0.21634 (6) | 0.96202 (6) | 0.0226 (2) | |
C1 | 0.8360 (3) | 0.3202 (2) | 0.8518 (2) | 0.0300 (10) | |
H1A | 0.7918 | 0.3109 | 0.8071 | 0.036* | |
H1B | 0.9130 | 0.3117 | 0.8386 | 0.036* | |
C2 | 0.8210 (4) | 0.4044 (2) | 0.8762 (3) | 0.0413 (11) | |
H2A | 0.7458 | 0.4125 | 0.8917 | 0.062* | |
H2B | 0.8379 | 0.4392 | 0.8350 | 0.062* | |
H2C | 0.8699 | 0.4155 | 0.9174 | 0.062* | |
C11 | 0.9634 (3) | 0.1431 (2) | 0.9067 (2) | 0.0244 (9) | |
C12 | 0.9538 (3) | 0.1404 (3) | 0.8308 (2) | 0.0347 (10) | |
H12 | 0.9089 | 0.1768 | 0.8060 | 0.042* | |
C13 | 1.0099 (4) | 0.0845 (3) | 0.7910 (3) | 0.0428 (12) | |
H13 | 1.0027 | 0.0826 | 0.7390 | 0.051* | |
C14 | 1.0760 (4) | 0.0317 (3) | 0.8262 (3) | 0.0398 (11) | |
H14 | 1.1155 | −0.0055 | 0.7984 | 0.048* | |
C15 | 1.0848 (4) | 0.0329 (3) | 0.9009 (3) | 0.0393 (11) | |
H15 | 1.1297 | −0.0041 | 0.9250 | 0.047* | |
C16 | 1.0283 (3) | 0.0879 (2) | 0.9421 (2) | 0.0301 (9) | |
H16 | 1.0339 | 0.0880 | 0.9942 | 0.036* | |
C21 | 0.9994 (3) | 0.2878 (2) | 0.9796 (2) | 0.0267 (9) | |
C22 | 1.0943 (3) | 0.2924 (3) | 0.9375 (3) | 0.0402 (11) | |
H22 | 1.1069 | 0.2561 | 0.8991 | 0.048* | |
C23 | 1.1695 (4) | 0.3501 (3) | 0.9521 (3) | 0.0532 (15) | |
H23 | 1.2336 | 0.3534 | 0.9232 | 0.064* | |
C24 | 1.1521 (4) | 0.4029 (3) | 1.0083 (3) | 0.0515 (14) | |
H24 | 1.2043 | 0.4423 | 1.0178 | 0.062* | |
C25 | 1.0602 (4) | 0.3988 (3) | 1.0502 (3) | 0.0471 (13) | |
H25 | 1.0482 | 0.4353 | 1.0885 | 0.057* | |
C26 | 0.9856 (4) | 0.3416 (3) | 1.0367 (3) | 0.0390 (11) | |
H26 | 0.9228 | 0.3382 | 1.0668 | 0.047* | |
O1 | 0.0875 (5) | 0.3175 (4) | 0.7631 (3) | 0.139 (3) | |
C31 | 0.1485 (8) | 0.3817 (6) | 0.7578 (4) | 0.134 (4) | |
H31A | 0.2149 | 0.3755 | 0.7879 | 0.161* | |
H31B | 0.1076 | 0.4269 | 0.7771 | 0.161* | |
C32 | 0.1791 (6) | 0.3963 (4) | 0.6793 (4) | 0.093 (2) | |
H32A | 0.1566 | 0.4488 | 0.6632 | 0.111* | |
H32B | 0.2582 | 0.3904 | 0.6718 | 0.111* | |
C33 | 0.1174 (7) | 0.3346 (4) | 0.6396 (4) | 0.099 (3) | |
H33A | 0.0610 | 0.3582 | 0.6078 | 0.119* | |
H33B | 0.1667 | 0.3033 | 0.6084 | 0.119* | |
C34 | 0.0669 (6) | 0.2854 (5) | 0.6968 (4) | 0.095 (2) | |
H34A | −0.0124 | 0.2821 | 0.6887 | 0.114* | |
H34B | 0.0973 | 0.2321 | 0.6947 | 0.114* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au | 0.02502 (8) | 0.02674 (8) | 0.02271 (8) | 0.00606 (7) | 0.00177 (7) | 0.00268 (7) |
Cl | 0.0369 (6) | 0.0436 (6) | 0.0253 (5) | 0.0084 (5) | 0.0066 (5) | 0.0081 (5) |
N | 0.0158 (16) | 0.0250 (17) | 0.0270 (16) | 0.0007 (14) | 0.0011 (13) | 0.0051 (14) |
P | 0.0190 (5) | 0.0254 (5) | 0.0234 (5) | 0.0038 (4) | −0.0002 (4) | 0.0010 (4) |
C1 | 0.026 (2) | 0.034 (2) | 0.031 (2) | 0.0036 (19) | 0.0055 (17) | 0.0080 (19) |
C2 | 0.046 (3) | 0.031 (2) | 0.046 (3) | −0.002 (2) | −0.002 (2) | 0.011 (2) |
C11 | 0.018 (2) | 0.024 (2) | 0.030 (2) | 0.0037 (16) | 0.0022 (17) | 0.0007 (17) |
C12 | 0.032 (2) | 0.040 (2) | 0.032 (2) | 0.009 (2) | 0.001 (2) | 0.003 (2) |
C13 | 0.050 (3) | 0.047 (3) | 0.032 (3) | 0.012 (2) | 0.009 (2) | −0.010 (2) |
C14 | 0.040 (3) | 0.038 (3) | 0.041 (3) | 0.014 (2) | 0.006 (2) | −0.009 (2) |
C15 | 0.032 (3) | 0.035 (3) | 0.051 (3) | 0.010 (2) | −0.003 (2) | 0.000 (2) |
C16 | 0.028 (2) | 0.030 (2) | 0.032 (2) | 0.0044 (18) | −0.0014 (19) | −0.0013 (19) |
C21 | 0.021 (2) | 0.030 (2) | 0.029 (2) | 0.0029 (18) | −0.0009 (17) | 0.0011 (19) |
C22 | 0.029 (2) | 0.047 (3) | 0.044 (3) | −0.003 (2) | 0.005 (2) | −0.011 (2) |
C23 | 0.028 (3) | 0.070 (4) | 0.062 (4) | −0.016 (2) | 0.009 (2) | −0.013 (3) |
C24 | 0.039 (3) | 0.056 (3) | 0.059 (3) | −0.023 (3) | −0.002 (2) | −0.009 (3) |
C25 | 0.042 (3) | 0.048 (3) | 0.051 (3) | −0.007 (2) | 0.004 (2) | −0.019 (2) |
C26 | 0.030 (2) | 0.047 (3) | 0.040 (3) | −0.006 (2) | 0.009 (2) | −0.001 (2) |
O1 | 0.142 (5) | 0.228 (7) | 0.048 (3) | −0.110 (5) | 0.010 (3) | −0.001 (4) |
C31 | 0.184 (10) | 0.148 (9) | 0.071 (6) | −0.072 (8) | 0.018 (6) | −0.011 (6) |
C32 | 0.090 (5) | 0.092 (5) | 0.096 (6) | −0.025 (4) | 0.018 (5) | 0.016 (5) |
C33 | 0.122 (6) | 0.125 (7) | 0.050 (4) | −0.060 (5) | −0.016 (4) | 0.019 (4) |
C34 | 0.095 (5) | 0.131 (6) | 0.059 (4) | −0.035 (5) | −0.005 (4) | 0.020 (4) |
Au—P | 2.2331 (11) | C21—C22 | 1.399 (6) |
Au—Cl | 2.3021 (10) | C21—C26 | 1.400 (6) |
Au—Aui | 3.1310 (5) | C22—C23 | 1.383 (6) |
N—Ni | 1.416 (6) | C22—H22 | 0.9500 |
N—C1 | 1.481 (5) | C23—C24 | 1.385 (7) |
N—P | 1.679 (3) | C23—H23 | 0.9500 |
P—C21 | 1.810 (4) | C24—C25 | 1.367 (6) |
P—C11 | 1.820 (4) | C24—H24 | 0.9500 |
C1—C2 | 1.526 (6) | C25—C26 | 1.369 (6) |
C1—H1A | 0.9900 | C25—H25 | 0.9500 |
C1—H1B | 0.9900 | C26—H26 | 0.9500 |
C2—H2A | 0.9800 | O1—C31 | 1.340 (9) |
C2—H2B | 0.9800 | O1—C34 | 1.349 (8) |
C2—H2C | 0.9800 | C31—C32 | 1.497 (9) |
C11—C12 | 1.386 (6) | C31—H31A | 0.9900 |
C11—C16 | 1.397 (5) | C31—H31B | 0.9900 |
C12—C13 | 1.388 (6) | C32—C33 | 1.491 (9) |
C12—H12 | 0.9500 | C32—H32A | 0.9900 |
C13—C14 | 1.377 (6) | C32—H32B | 0.9900 |
C13—H13 | 0.9500 | C33—C34 | 1.479 (8) |
C14—C15 | 1.361 (6) | C33—H33A | 0.9900 |
C14—H14 | 0.9500 | C33—H33B | 0.9900 |
C15—C16 | 1.394 (6) | C34—H34A | 0.9900 |
C15—H15 | 0.9500 | C34—H34B | 0.9900 |
C16—H16 | 0.9500 | ||
P—Au—Cl | 179.22 (4) | C22—C21—P | 122.5 (3) |
P—Au—Aui | 86.37 (3) | C26—C21—P | 119.5 (3) |
Cl—Au—Aui | 94.01 (3) | C23—C22—C21 | 119.7 (4) |
Ni—N—C1 | 117.4 (3) | C23—C22—H22 | 120.1 |
Ni—N—P | 118.4 (3) | C21—C22—H22 | 120.1 |
C1—N—P | 123.1 (2) | C22—C23—C24 | 120.6 (5) |
N—P—C21 | 104.37 (17) | C22—C23—H23 | 119.7 |
N—P—C11 | 108.89 (18) | C24—C23—H23 | 119.7 |
C21—P—C11 | 103.71 (18) | C25—C24—C23 | 120.3 (5) |
N—P—Au | 110.68 (11) | C25—C24—H24 | 119.8 |
C21—P—Au | 113.12 (13) | C23—C24—H24 | 119.8 |
C11—P—Au | 115.30 (14) | C24—C25—C26 | 119.6 (5) |
N—C1—C2 | 113.1 (3) | C24—C25—H25 | 120.2 |
N—C1—H1A | 109.0 | C26—C25—H25 | 120.2 |
C2—C1—H1A | 109.0 | C25—C26—C21 | 121.7 (4) |
N—C1—H1B | 109.0 | C25—C26—H26 | 119.1 |
C2—C1—H1B | 109.0 | C21—C26—H26 | 119.1 |
H1A—C1—H1B | 107.8 | C31—O1—C34 | 112.3 (6) |
C1—C2—H2A | 109.5 | O1—C31—C32 | 110.3 (7) |
C1—C2—H2B | 109.5 | O1—C31—H31A | 109.6 |
H2A—C2—H2B | 109.5 | C32—C31—H31A | 109.6 |
C1—C2—H2C | 109.5 | O1—C31—H31B | 109.6 |
H2A—C2—H2C | 109.5 | C32—C31—H31B | 109.6 |
H2B—C2—H2C | 109.5 | H31A—C31—H31B | 108.1 |
C12—C11—C16 | 118.9 (4) | C33—C32—C31 | 102.4 (6) |
C12—C11—P | 122.2 (3) | C33—C32—H32A | 111.3 |
C16—C11—P | 118.8 (3) | C31—C32—H32A | 111.3 |
C11—C12—C13 | 120.0 (4) | C33—C32—H32B | 111.3 |
C11—C12—H12 | 120.0 | C31—C32—H32B | 111.3 |
C13—C12—H12 | 120.0 | H32A—C32—H32B | 109.2 |
C14—C13—C12 | 120.6 (4) | C34—C33—C32 | 106.3 (6) |
C14—C13—H13 | 119.7 | C34—C33—H33A | 110.5 |
C12—C13—H13 | 119.7 | C32—C33—H33A | 110.5 |
C15—C14—C13 | 120.0 (4) | C34—C33—H33B | 110.5 |
C15—C14—H14 | 120.0 | C32—C33—H33B | 110.5 |
C13—C14—H14 | 120.0 | H33A—C33—H33B | 108.7 |
C14—C15—C16 | 120.4 (4) | O1—C34—C33 | 108.3 (6) |
C14—C15—H15 | 119.8 | O1—C34—H34A | 110.0 |
C16—C15—H15 | 119.8 | C33—C34—H34A | 110.0 |
C15—C16—C11 | 120.0 (4) | O1—C34—H34B | 110.0 |
C15—C16—H16 | 120.0 | C33—C34—H34B | 110.0 |
C11—C16—H16 | 120.0 | H34A—C34—H34B | 108.4 |
C22—C21—C26 | 118.0 (4) | ||
Ni—N—P—C21 | −155.3 (2) | C14—C15—C16—C11 | −0.9 (7) |
C1—N—P—C21 | 37.0 (3) | C12—C11—C16—C15 | 1.9 (6) |
Ni—N—P—C11 | 94.4 (3) | P—C11—C16—C15 | −177.7 (3) |
C1—N—P—C11 | −73.3 (3) | N—P—C21—C22 | −95.7 (4) |
Ni—N—P—Au | −33.3 (3) | C11—P—C21—C22 | 18.3 (4) |
C1—N—P—Au | 159.0 (3) | Au—P—C21—C22 | 144.0 (3) |
Aui—Au—P—N | −38.27 (13) | N—P—C21—C26 | 83.6 (4) |
Aui—Au—P—C21 | 78.44 (14) | C11—P—C21—C26 | −162.4 (3) |
Aui—Au—P—C11 | −162.41 (14) | Au—P—C21—C26 | −36.8 (4) |
Ni—N—C1—C2 | 90.6 (4) | C26—C21—C22—C23 | −1.4 (7) |
P—N—C1—C2 | −101.6 (4) | P—C21—C22—C23 | 177.8 (4) |
N—P—C11—C12 | 11.5 (4) | C21—C22—C23—C24 | 0.5 (8) |
C21—P—C11—C12 | −99.2 (4) | C22—C23—C24—C25 | 0.0 (9) |
Au—P—C11—C12 | 136.5 (3) | C23—C24—C25—C26 | 0.5 (8) |
N—P—C11—C16 | −168.9 (3) | C24—C25—C26—C21 | −1.6 (8) |
C21—P—C11—C16 | 80.4 (3) | C22—C21—C26—C25 | 2.0 (7) |
Au—P—C11—C16 | −43.8 (4) | P—C21—C26—C25 | −177.3 (4) |
C16—C11—C12—C13 | −1.2 (6) | C34—O1—C31—C32 | −2.4 (12) |
P—C11—C12—C13 | 178.4 (3) | O1—C31—C32—C33 | 5.2 (11) |
C11—C12—C13—C14 | −0.6 (7) | C31—C32—C33—C34 | −5.8 (9) |
C12—C13—C14—C15 | 1.6 (7) | C31—O1—C34—C33 | −1.6 (11) |
C13—C14—C15—C16 | −0.8 (7) | C32—C33—C34—O1 | 4.9 (10) |
Symmetry code: (i) −x+3/2, −y+1/2, z. |
Experimental details
Crystal data | |
Chemical formula | [Au2Cl2(C28H30N2P2)]·2C4H8O |
Mr | 1065.52 |
Crystal system, space group | Orthorhombic, Pccn |
Temperature (K) | 173 |
a, b, c (Å) | 12.3275 (18), 17.200 (3), 18.173 (3) |
V (Å3) | 3853.4 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 7.86 |
Crystal size (mm) | 0.48 × 0.23 × 0.14 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Integration (SADABS; Bruker, 1999) |
Tmin, Tmax | 0.116, 0.406 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 23024, 4199, 3256 |
Rint | 0.045 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.052, 1.06 |
No. of reflections | 4199 |
No. of parameters | 209 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.52, −1.22 |
Computer programs: SMART-NT (Bruker, 1998), SAINT-Plus (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997) and Mercury (Macrae et al., 2008), WinGX (Farrugia, 1999).
Gold(I) forms an almost linear complex with a P—Au—Cl angles of 179.22 (4) °. The Au—Au distance of the complex is 3.131 (5) Å and is intramolecular. This is well within the range of aurophilic interactions as discribed by Holleman et al. as being normally between 2.7 Å and 3.4 Å. Other bond lengths are within expected ranges.
The molecule readilly crystalizes out of tetrahydrofuran (THF) and also includes this solvent in the crystal lattice. The molecule exhibits columns of head-to-tail complexes forming channels filled with THF. Intermolecular short contacts of 2.822 Å and 2.835 Å are displayed between Cl and H(1a) and Cl and H(14), respectively (Figure 2). The Cl—H(1a) interaction can be seen on the head-to-tail arranged complexes in a column between chlorines and adjacent hydrogen atoms situated on the ethyl substituted hydrazine bridge. The Cl—H(14) interaction occurs between chlorines and H atoms situated on a phenyl ring in close proximity. Hydrogen bonding distances between the THF O(1) atom and H(1 b) and H(22) are observed to be 2.553 Å and 2.698 Å, respectively.