Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803006834/lh6047sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803006834/lh6047Isup2.hkl |
CCDC reference: 209904
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.013 Å
- R factor = 0.041
- wR factor = 0.110
- Data-to-parameter ratio = 14.2
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C(2) - C(3) = 1.43 Ang. PLAT_601 Alert C Structure Contains Solvent Accessible VOIDS of 36.00 A 3
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
The starting compounds Pt(dmbpy)(C2Ph)2 (Chan et al., 2001) and [Ag(PPh3)2(MeCN)](SbF6) were prepared according to literature procedures (Bachman et al., 1998). Pt(dmbpy)(C2Ph)2 and [Ag(PPh3)2(MeCN)](SbF6) were reacted, in an equimolar ratio, in dichloromethane under anaerobic conditions for 24 h. The solvent was then reduced in vacuo. Well shaped yellow crystals suitable for X-ray diffraction analysis were grown by slow diffusion of diethyl ether into the dichloromethane solution.
All H atoms were included in calculated positions with C—H distances of 0.93 and 0.96 Å (methyl). They were included in the refinement in riding-motion approximation, with Uiso = 1.2Ueq (1.5Ueq for methyl) of the carrier atom.
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. A view of the compound with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. |
[Pt(C8H5)(C18H15P)(C12H12N2)](SbF6) | F(000) = 1888 |
Mr = 978.47 | Dx = 1.814 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 4988 reflections |
a = 14.4131 (4) Å | θ = 1.5–25.1° |
b = 10.1848 (2) Å | µ = 4.76 mm−1 |
c = 24.7099 (7) Å | T = 293 K |
β = 98.915 (1)° | Block, yellow |
V = 3583.46 (16) Å3 | 0.50 × 0.30 × 0.25 mm |
Z = 4 |
Siemens SMART CCD diffractometer | 6291 independent reflections |
Radiation source: fine-focus sealed tube | 4473 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
ω scans | θmax = 25.1°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −7→17 |
Tmin = 0.194, Tmax = 0.304 | k = −9→12 |
10524 measured reflections | l = −29→29 |
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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.110 | H-atom parameters constrained |
S = 1.19 | w = 1/[σ2(Fo2) + (0.0387P)2 + 9.8193P] where P = (Fo2 + 2Fc2)/3 |
6291 reflections | (Δ/σ)max = 0.002 |
442 parameters | Δρmax = 1.04 e Å−3 |
0 restraints | Δρmin = −0.61 e Å−3 |
[Pt(C8H5)(C18H15P)(C12H12N2)](SbF6) | V = 3583.46 (16) Å3 |
Mr = 978.47 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 14.4131 (4) Å | µ = 4.76 mm−1 |
b = 10.1848 (2) Å | T = 293 K |
c = 24.7099 (7) Å | 0.50 × 0.30 × 0.25 mm |
β = 98.915 (1)° |
Siemens SMART CCD diffractometer | 6291 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4473 reflections with I > 2σ(I) |
Tmin = 0.194, Tmax = 0.304 | Rint = 0.024 |
10524 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.110 | H-atom parameters constrained |
S = 1.19 | Δρmax = 1.04 e Å−3 |
6291 reflections | Δρmin = −0.61 e Å−3 |
442 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 | ||
Pt | 0.11648 (2) | 0.00002 (3) | 0.094070 (11) | 0.04068 (11) | |
Sb | 0.49147 (5) | 0.18053 (7) | 0.10878 (3) | 0.06338 (19) | |
P | 0.06876 (14) | −0.0455 (2) | 0.17434 (8) | 0.0424 (5) | |
F1 | 0.4859 (4) | 0.0352 (6) | 0.0637 (3) | 0.101 (2) | |
F2 | 0.6135 (6) | 0.1462 (11) | 0.1340 (6) | 0.227 (7) | |
F3 | 0.5005 (5) | 0.3269 (7) | 0.1539 (2) | 0.104 (2) | |
F4 | 0.3707 (6) | 0.2193 (13) | 0.0842 (5) | 0.219 (6) | |
F5 | 0.4544 (11) | 0.0870 (10) | 0.1626 (4) | 0.229 (7) | |
F6 | 0.5241 (11) | 0.2795 (10) | 0.0542 (4) | 0.219 (6) | |
N1 | 0.1700 (4) | 0.0471 (6) | 0.0236 (3) | 0.0418 (15) | |
N2 | 0.2270 (4) | −0.1346 (6) | 0.0971 (2) | 0.0416 (15) | |
C1 | 0.0150 (6) | 0.1284 (8) | 0.0793 (3) | 0.0470 (19) | |
C2 | −0.0466 (6) | 0.2070 (8) | 0.0645 (3) | 0.050 (2) | |
C3 | −0.1147 (5) | 0.3057 (8) | 0.0450 (3) | 0.047 (2) | |
C4 | −0.1952 (6) | 0.3232 (9) | 0.0678 (4) | 0.063 (2) | |
H4A | −0.2067 | 0.2677 | 0.0959 | 0.075* | |
C5 | −0.2598 (7) | 0.4219 (12) | 0.0500 (5) | 0.081 (3) | |
H5A | −0.3133 | 0.4342 | 0.0661 | 0.098* | |
C6 | −0.2414 (9) | 0.5006 (11) | 0.0074 (6) | 0.094 (4) | |
H6A | −0.2845 | 0.5656 | −0.0056 | 0.113* | |
C7 | −0.1622 (10) | 0.4866 (11) | −0.0166 (5) | 0.084 (3) | |
H7A | −0.1513 | 0.5414 | −0.0450 | 0.101* | |
C8 | −0.0995 (7) | 0.3899 (9) | 0.0026 (4) | 0.063 (2) | |
H8A | −0.0453 | 0.3801 | −0.0131 | 0.076* | |
C11 | 0.1695 (5) | −0.0594 (8) | 0.2290 (3) | 0.0410 (18) | |
C12 | 0.1662 (6) | −0.1371 (8) | 0.2743 (3) | 0.051 (2) | |
H12A | 0.1114 | −0.1825 | 0.2776 | 0.061* | |
C13 | 0.2437 (6) | −0.1483 (9) | 0.3150 (3) | 0.057 (2) | |
H13A | 0.2403 | −0.1996 | 0.3457 | 0.069* | |
C14 | 0.3252 (6) | −0.0837 (9) | 0.3098 (4) | 0.057 (2) | |
H14A | 0.3775 | −0.0924 | 0.3368 | 0.069* | |
C15 | 0.3297 (6) | −0.0068 (9) | 0.2654 (4) | 0.063 (2) | |
H15A | 0.3849 | 0.0381 | 0.2624 | 0.075* | |
C16 | 0.2525 (6) | 0.0054 (8) | 0.2242 (3) | 0.054 (2) | |
H16A | 0.2565 | 0.0569 | 0.1936 | 0.065* | |
C21 | −0.0079 (6) | 0.0718 (8) | 0.2017 (3) | 0.049 (2) | |
C22 | 0.0280 (7) | 0.1662 (9) | 0.2385 (4) | 0.063 (2) | |
H22A | 0.0926 | 0.1718 | 0.2494 | 0.076* | |
C23 | −0.0314 (9) | 0.2547 (11) | 0.2598 (4) | 0.084 (3) | |
H23A | −0.0064 | 0.3178 | 0.2851 | 0.101* | |
C24 | −0.1256 (9) | 0.2478 (12) | 0.2434 (5) | 0.081 (3) | |
H24A | −0.1649 | 0.3068 | 0.2574 | 0.097* | |
C25 | −0.1635 (7) | 0.1547 (12) | 0.2062 (5) | 0.080 (3) | |
H25A | −0.2282 | 0.1497 | 0.1956 | 0.095* | |
C26 | −0.1043 (6) | 0.0682 (10) | 0.1846 (4) | 0.066 (3) | |
H26A | −0.1295 | 0.0071 | 0.1584 | 0.079* | |
C31 | 0.0069 (5) | −0.2006 (8) | 0.1732 (3) | 0.0453 (19) | |
C32 | −0.0498 (6) | −0.2332 (10) | 0.2123 (4) | 0.061 (2) | |
H32A | −0.0575 | −0.1739 | 0.2399 | 0.073* | |
C33 | −0.0944 (6) | −0.3540 (10) | 0.2100 (4) | 0.067 (3) | |
H33A | −0.1318 | −0.3754 | 0.2361 | 0.081* | |
C34 | −0.0838 (7) | −0.4421 (11) | 0.1695 (4) | 0.070 (3) | |
H34A | −0.1132 | −0.5235 | 0.1687 | 0.084* | |
C35 | −0.0305 (6) | −0.4107 (9) | 0.1308 (4) | 0.061 (2) | |
H35A | −0.0246 | −0.4700 | 0.1029 | 0.073* | |
C36 | 0.0155 (6) | −0.2903 (8) | 0.1325 (3) | 0.050 (2) | |
H36A | 0.0524 | −0.2702 | 0.1059 | 0.060* | |
C42 | 0.2498 (5) | −0.0163 (7) | 0.0162 (3) | 0.0397 (18) | |
C43 | 0.2982 (6) | 0.0174 (8) | −0.0258 (3) | 0.052 (2) | |
H43A | 0.3529 | −0.0274 | −0.0299 | 0.063* | |
C44 | 0.2660 (6) | 0.1170 (9) | −0.0618 (3) | 0.050 (2) | |
C45 | 0.1851 (6) | 0.1797 (9) | −0.0541 (3) | 0.053 (2) | |
H45A | 0.1614 | 0.2475 | −0.0774 | 0.064* | |
C46 | 0.1388 (6) | 0.1427 (8) | −0.0120 (3) | 0.052 (2) | |
H46A | 0.0834 | 0.1858 | −0.0080 | 0.063* | |
C47 | 0.3179 (7) | 0.1593 (11) | −0.1071 (4) | 0.078 (3) | |
H47A | 0.3721 | 0.1045 | −0.1072 | 0.118* | |
H47B | 0.3374 | 0.2490 | −0.1015 | 0.118* | |
H47C | 0.2774 | 0.1513 | −0.1417 | 0.118* | |
C52 | 0.2799 (5) | −0.1199 (7) | 0.0564 (3) | 0.0433 (18) | |
C53 | 0.3537 (5) | −0.2008 (8) | 0.0522 (4) | 0.051 (2) | |
H53A | 0.3887 | −0.1869 | 0.0241 | 0.062* | |
C54 | 0.3782 (6) | −0.3034 (8) | 0.0887 (4) | 0.056 (2) | |
C55 | 0.3234 (6) | −0.3164 (9) | 0.1299 (4) | 0.055 (2) | |
H55A | 0.3367 | −0.3830 | 0.1557 | 0.066* | |
C56 | 0.2498 (6) | −0.2325 (8) | 0.1332 (3) | 0.051 (2) | |
H56A | 0.2146 | −0.2438 | 0.1614 | 0.061* | |
C57 | 0.4592 (7) | −0.3934 (10) | 0.0842 (5) | 0.076 (3) | |
H57A | 0.4650 | −0.4569 | 0.1132 | 0.114* | |
H57B | 0.5161 | −0.3431 | 0.0869 | 0.114* | |
H57C | 0.4484 | −0.4379 | 0.0495 | 0.114* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt | 0.04262 (17) | 0.04339 (18) | 0.03631 (16) | −0.00069 (16) | 0.00701 (11) | 0.00109 (15) |
Sb | 0.0604 (4) | 0.0776 (4) | 0.0557 (4) | −0.0025 (3) | 0.0203 (3) | −0.0065 (4) |
P | 0.0424 (11) | 0.0477 (12) | 0.0370 (11) | −0.0083 (9) | 0.0059 (9) | −0.0027 (9) |
F1 | 0.080 (4) | 0.101 (5) | 0.119 (5) | −0.007 (3) | 0.011 (4) | −0.046 (4) |
F2 | 0.090 (6) | 0.221 (11) | 0.335 (15) | 0.051 (6) | −0.076 (7) | −0.166 (11) |
F3 | 0.142 (6) | 0.099 (5) | 0.076 (4) | −0.014 (4) | 0.036 (4) | −0.026 (4) |
F4 | 0.097 (6) | 0.292 (14) | 0.250 (12) | 0.068 (7) | −0.030 (7) | −0.151 (11) |
F5 | 0.43 (2) | 0.149 (9) | 0.139 (8) | −0.116 (11) | 0.137 (11) | 0.009 (7) |
F6 | 0.412 (18) | 0.148 (8) | 0.132 (8) | −0.053 (10) | 0.159 (10) | −0.022 (6) |
N1 | 0.042 (4) | 0.046 (4) | 0.039 (4) | 0.002 (3) | 0.009 (3) | 0.006 (3) |
N2 | 0.045 (4) | 0.043 (4) | 0.036 (3) | −0.001 (3) | 0.006 (3) | −0.002 (3) |
C1 | 0.053 (5) | 0.051 (5) | 0.038 (4) | −0.003 (4) | 0.011 (4) | −0.004 (4) |
C2 | 0.054 (5) | 0.045 (5) | 0.051 (5) | 0.001 (4) | 0.012 (4) | −0.005 (4) |
C3 | 0.042 (4) | 0.050 (5) | 0.046 (5) | 0.003 (4) | −0.004 (4) | −0.008 (4) |
C4 | 0.049 (5) | 0.054 (6) | 0.084 (7) | 0.002 (5) | 0.005 (5) | −0.006 (5) |
C5 | 0.056 (6) | 0.078 (8) | 0.106 (9) | 0.008 (6) | 0.001 (6) | −0.016 (7) |
C6 | 0.091 (9) | 0.055 (6) | 0.119 (10) | 0.014 (7) | −0.044 (8) | −0.017 (8) |
C7 | 0.104 (9) | 0.068 (7) | 0.072 (7) | 0.000 (7) | −0.011 (7) | 0.005 (6) |
C8 | 0.070 (6) | 0.063 (6) | 0.055 (6) | 0.003 (5) | 0.003 (5) | −0.003 (5) |
C11 | 0.044 (4) | 0.040 (4) | 0.040 (4) | −0.008 (4) | 0.008 (3) | −0.002 (4) |
C12 | 0.053 (5) | 0.059 (5) | 0.042 (5) | −0.017 (4) | 0.010 (4) | −0.002 (4) |
C13 | 0.063 (6) | 0.071 (6) | 0.038 (5) | −0.005 (5) | 0.006 (4) | 0.004 (4) |
C14 | 0.049 (5) | 0.067 (6) | 0.052 (5) | −0.008 (5) | −0.006 (4) | 0.004 (5) |
C15 | 0.049 (5) | 0.060 (6) | 0.079 (6) | −0.019 (5) | 0.009 (5) | −0.002 (6) |
C16 | 0.059 (5) | 0.053 (5) | 0.048 (5) | −0.014 (5) | 0.004 (4) | 0.002 (5) |
C21 | 0.053 (5) | 0.052 (5) | 0.046 (5) | 0.003 (4) | 0.022 (4) | 0.005 (4) |
C22 | 0.072 (6) | 0.056 (6) | 0.059 (6) | −0.001 (5) | 0.004 (5) | −0.010 (5) |
C23 | 0.121 (10) | 0.064 (7) | 0.068 (7) | 0.008 (7) | 0.017 (7) | −0.012 (6) |
C24 | 0.083 (8) | 0.091 (8) | 0.075 (8) | 0.020 (7) | 0.036 (6) | 0.004 (7) |
C25 | 0.050 (6) | 0.111 (9) | 0.083 (7) | 0.013 (6) | 0.029 (5) | 0.005 (7) |
C26 | 0.049 (5) | 0.077 (7) | 0.072 (6) | −0.005 (5) | 0.016 (5) | −0.008 (6) |
C31 | 0.044 (4) | 0.049 (5) | 0.040 (4) | −0.006 (4) | −0.001 (4) | 0.002 (4) |
C32 | 0.057 (6) | 0.072 (6) | 0.051 (5) | −0.020 (5) | 0.002 (4) | −0.006 (5) |
C33 | 0.057 (6) | 0.083 (7) | 0.060 (6) | −0.028 (5) | 0.004 (5) | 0.022 (6) |
C34 | 0.075 (7) | 0.060 (6) | 0.065 (7) | −0.022 (5) | −0.017 (5) | 0.009 (6) |
C35 | 0.069 (6) | 0.052 (6) | 0.053 (5) | −0.005 (5) | −0.017 (5) | 0.000 (4) |
C36 | 0.049 (5) | 0.049 (5) | 0.047 (5) | −0.006 (4) | −0.005 (4) | −0.001 (4) |
C42 | 0.038 (4) | 0.048 (5) | 0.033 (4) | 0.001 (4) | 0.005 (3) | −0.003 (4) |
C43 | 0.049 (5) | 0.059 (6) | 0.051 (5) | 0.008 (4) | 0.016 (4) | 0.003 (4) |
C44 | 0.052 (5) | 0.058 (5) | 0.040 (5) | 0.004 (4) | 0.004 (4) | 0.006 (4) |
C45 | 0.055 (5) | 0.059 (5) | 0.046 (5) | 0.007 (4) | 0.008 (4) | 0.022 (4) |
C46 | 0.050 (5) | 0.056 (5) | 0.052 (5) | 0.010 (4) | 0.011 (4) | 0.009 (4) |
C47 | 0.068 (6) | 0.096 (8) | 0.078 (7) | 0.010 (6) | 0.036 (5) | 0.040 (6) |
C52 | 0.045 (4) | 0.039 (4) | 0.044 (4) | −0.005 (4) | 0.001 (4) | 0.008 (4) |
C53 | 0.041 (4) | 0.056 (5) | 0.059 (5) | 0.010 (4) | 0.014 (4) | 0.003 (4) |
C54 | 0.058 (5) | 0.044 (5) | 0.063 (6) | 0.007 (4) | −0.003 (4) | 0.001 (5) |
C55 | 0.060 (5) | 0.045 (5) | 0.056 (5) | 0.001 (4) | −0.003 (4) | 0.004 (4) |
C56 | 0.049 (5) | 0.053 (5) | 0.050 (5) | 0.001 (4) | 0.004 (4) | 0.008 (4) |
C57 | 0.072 (7) | 0.057 (6) | 0.097 (8) | 0.026 (5) | 0.004 (6) | 0.009 (6) |
Pt—C1 | 1.954 (9) | C22—C23 | 1.401 (13) |
Pt—N1 | 2.068 (6) | C22—H22A | 0.9300 |
Pt—N2 | 2.094 (6) | C23—C24 | 1.357 (15) |
Pt—P | 2.246 (2) | C23—H23A | 0.9300 |
Sb—F5 | 1.783 (8) | C24—C25 | 1.372 (15) |
Sb—F4 | 1.797 (8) | C24—H24A | 0.9300 |
Sb—F6 | 1.803 (9) | C25—C26 | 1.389 (13) |
Sb—F2 | 1.807 (7) | C25—H25A | 0.9300 |
Sb—F1 | 1.847 (6) | C26—H26A | 0.9300 |
Sb—F3 | 1.854 (6) | C31—C36 | 1.378 (11) |
P—C31 | 1.812 (8) | C31—C32 | 1.400 (11) |
P—C21 | 1.827 (8) | C32—C33 | 1.385 (12) |
P—C11 | 1.828 (8) | C32—H32A | 0.9300 |
N1—C46 | 1.341 (10) | C33—C34 | 1.369 (14) |
N1—C42 | 1.356 (9) | C33—H33A | 0.9300 |
N2—C56 | 1.343 (9) | C34—C35 | 1.356 (13) |
N2—C52 | 1.362 (9) | C34—H34A | 0.9300 |
C1—C2 | 1.209 (11) | C35—C36 | 1.391 (11) |
C2—C3 | 1.435 (11) | C35—H35A | 0.9300 |
C3—C4 | 1.378 (11) | C36—H36A | 0.9300 |
C3—C8 | 1.397 (12) | C42—C43 | 1.380 (11) |
C4—C5 | 1.395 (13) | C42—C52 | 1.468 (10) |
C4—H4A | 0.9300 | C43—C44 | 1.381 (11) |
C5—C6 | 1.381 (17) | C43—H43A | 0.9300 |
C5—H5A | 0.9300 | C44—C45 | 1.368 (11) |
C6—C7 | 1.373 (18) | C44—C47 | 1.505 (11) |
C6—H6A | 0.9300 | C45—C46 | 1.372 (11) |
C7—C8 | 1.370 (14) | C45—H45A | 0.9300 |
C7—H7A | 0.9300 | C46—H46A | 0.9300 |
C8—H8A | 0.9300 | C47—H47A | 0.9600 |
C11—C12 | 1.378 (10) | C47—H47B | 0.9600 |
C11—C16 | 1.387 (11) | C47—H47C | 0.9600 |
C12—C13 | 1.387 (11) | C52—C53 | 1.363 (10) |
C12—H12A | 0.9300 | C53—C54 | 1.390 (11) |
C13—C14 | 1.370 (11) | C53—H53A | 0.9300 |
C13—H13A | 0.9300 | C54—C55 | 1.387 (12) |
C14—C15 | 1.359 (12) | C54—C57 | 1.503 (12) |
C14—H14A | 0.9300 | C55—C56 | 1.375 (11) |
C15—C16 | 1.392 (12) | C55—H55A | 0.9300 |
C15—H15A | 0.9300 | C56—H56A | 0.9300 |
C16—H16A | 0.9300 | C57—H57A | 0.9600 |
C21—C22 | 1.367 (12) | C57—H57B | 0.9600 |
C21—C26 | 1.389 (12) | C57—H57C | 0.9600 |
C1—Pt—N1 | 93.0 (3) | C21—C22—H22A | 119.6 |
C1—Pt—N2 | 171.2 (3) | C23—C22—H22A | 119.6 |
N1—Pt—N2 | 78.6 (2) | C24—C23—C22 | 119.7 (10) |
C1—Pt—P | 88.9 (2) | C24—C23—H23A | 120.1 |
N1—Pt—P | 175.58 (18) | C22—C23—H23A | 120.1 |
N2—Pt—P | 99.68 (18) | C23—C24—C25 | 120.8 (10) |
F5—Sb—F4 | 89.0 (7) | C23—C24—H24A | 119.6 |
F5—Sb—F6 | 177.4 (7) | C25—C24—H24A | 119.6 |
F4—Sb—F6 | 88.6 (7) | C24—C25—C26 | 119.4 (10) |
F5—Sb—F2 | 91.6 (7) | C24—C25—H25A | 120.3 |
F4—Sb—F2 | 178.4 (5) | C26—C25—H25A | 120.3 |
F6—Sb—F2 | 90.7 (7) | C21—C26—C25 | 120.7 (10) |
F5—Sb—F1 | 91.8 (4) | C21—C26—H26A | 119.6 |
F4—Sb—F1 | 91.3 (4) | C25—C26—H26A | 119.6 |
F6—Sb—F1 | 89.3 (4) | C36—C31—C32 | 118.4 (8) |
F2—Sb—F1 | 90.1 (4) | C36—C31—P | 119.3 (6) |
F5—Sb—F3 | 89.0 (4) | C32—C31—P | 122.3 (6) |
F4—Sb—F3 | 90.0 (4) | C33—C32—C31 | 119.9 (9) |
F6—Sb—F3 | 89.9 (4) | C33—C32—H32A | 120.0 |
F2—Sb—F3 | 88.5 (4) | C31—C32—H32A | 120.0 |
F1—Sb—F3 | 178.4 (3) | C34—C33—C32 | 120.6 (9) |
C31—P—C21 | 104.6 (4) | C34—C33—H33A | 119.7 |
C31—P—C11 | 106.1 (4) | C32—C33—H33A | 119.7 |
C21—P—C11 | 103.5 (4) | C35—C34—C33 | 120.0 (9) |
C31—P—Pt | 112.5 (3) | C35—C34—H34A | 120.0 |
C21—P—Pt | 118.6 (3) | C33—C34—H34A | 120.0 |
C11—P—Pt | 110.6 (3) | C34—C35—C36 | 120.4 (9) |
C46—N1—C42 | 117.6 (7) | C34—C35—H35A | 119.8 |
C46—N1—Pt | 126.1 (5) | C36—C35—H35A | 119.8 |
C42—N1—Pt | 116.0 (5) | C31—C36—C35 | 120.7 (8) |
C56—N2—C52 | 117.7 (7) | C31—C36—H36A | 119.7 |
C56—N2—Pt | 128.0 (5) | C35—C36—H36A | 119.7 |
C52—N2—Pt | 114.2 (5) | N1—C42—C43 | 121.4 (7) |
C2—C1—Pt | 173.2 (7) | N1—C42—C52 | 114.8 (7) |
C1—C2—C3 | 175.7 (9) | C43—C42—C52 | 123.8 (7) |
C4—C3—C8 | 117.9 (8) | C42—C43—C44 | 120.5 (8) |
C4—C3—C2 | 121.9 (8) | C42—C43—H43A | 119.7 |
C8—C3—C2 | 120.2 (8) | C44—C43—H43A | 119.7 |
C3—C4—C5 | 121.8 (10) | C45—C44—C43 | 117.5 (8) |
C3—C4—H4A | 119.1 | C45—C44—C47 | 120.2 (8) |
C5—C4—H4A | 119.1 | C43—C44—C47 | 122.2 (8) |
C6—C5—C4 | 117.5 (11) | C44—C45—C46 | 120.1 (8) |
C6—C5—H5A | 121.3 | C44—C45—H45A | 119.9 |
C4—C5—H5A | 121.3 | C46—C45—H45A | 119.9 |
C7—C6—C5 | 122.6 (11) | N1—C46—C45 | 122.9 (8) |
C7—C6—H6A | 118.7 | N1—C46—H46A | 118.6 |
C5—C6—H6A | 118.7 | C45—C46—H46A | 118.6 |
C8—C7—C6 | 118.3 (11) | C44—C47—H47A | 109.5 |
C8—C7—H7A | 120.8 | C44—C47—H47B | 109.5 |
C6—C7—H7A | 120.8 | H47A—C47—H47B | 109.5 |
C7—C8—C3 | 121.9 (10) | C44—C47—H47C | 109.5 |
C7—C8—H8A | 119.1 | H47A—C47—H47C | 109.5 |
C3—C8—H8A | 119.1 | H47B—C47—H47C | 109.5 |
C12—C11—C16 | 118.7 (7) | N2—C52—C53 | 121.5 (7) |
C12—C11—P | 121.4 (6) | N2—C52—C42 | 116.0 (7) |
C16—C11—P | 119.8 (6) | C53—C52—C42 | 122.4 (7) |
C11—C12—C13 | 120.7 (8) | C52—C53—C54 | 121.9 (8) |
C11—C12—H12A | 119.6 | C52—C53—H53A | 119.1 |
C13—C12—H12A | 119.6 | C54—C53—H53A | 119.1 |
C14—C13—C12 | 119.9 (8) | C55—C54—C53 | 115.6 (8) |
C14—C13—H13A | 120.0 | C55—C54—C57 | 122.3 (8) |
C12—C13—H13A | 120.0 | C53—C54—C57 | 122.2 (9) |
C15—C14—C13 | 120.1 (8) | C56—C55—C54 | 121.1 (8) |
C15—C14—H14A | 120.0 | C56—C55—H55A | 119.4 |
C13—C14—H14A | 120.0 | C54—C55—H55A | 119.4 |
C14—C15—C16 | 120.5 (8) | N2—C56—C55 | 122.2 (8) |
C14—C15—H15A | 119.7 | N2—C56—H56A | 118.9 |
C16—C15—H15A | 119.7 | C55—C56—H56A | 118.9 |
C11—C16—C15 | 119.9 (8) | C54—C57—H57A | 109.5 |
C11—C16—H16A | 120.0 | C54—C57—H57B | 109.5 |
C15—C16—H16A | 120.0 | H57A—C57—H57B | 109.5 |
C22—C21—C26 | 118.6 (8) | C54—C57—H57C | 109.5 |
C22—C21—P | 121.2 (7) | H57A—C57—H57C | 109.5 |
C26—C21—P | 120.2 (7) | H57B—C57—H57C | 109.5 |
C21—C22—C23 | 120.8 (10) |
Experimental details
Crystal data | |
Chemical formula | [Pt(C8H5)(C18H15P)(C12H12N2)](SbF6) |
Mr | 978.47 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 14.4131 (4), 10.1848 (2), 24.7099 (7) |
β (°) | 98.915 (1) |
V (Å3) | 3583.46 (16) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.76 |
Crystal size (mm) | 0.50 × 0.30 × 0.25 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.194, 0.304 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10524, 6291, 4473 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.110, 1.19 |
No. of reflections | 6291 |
No. of parameters | 442 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.04, −0.61 |
Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens, 1994), XPREP (Siemens, 1994), SHELXTL (Siemens, 1994), SHELXTL.
Pt—C1 | 1.954 (9) | Pt—N2 | 2.094 (6) |
Pt—N1 | 2.068 (6) | Pt—P | 2.246 (2) |
C1—Pt—N1 | 93.0 (3) | C1—Pt—P | 88.9 (2) |
C1—Pt—N2 | 171.2 (3) | N1—Pt—P | 175.58 (18) |
N1—Pt—N2 | 78.6 (2) | N2—Pt—P | 99.68 (18) |
Transition metal acetylide complexes are of considerable interest because of their potential applications in many fields of materials chemistry, including luminiscent materials and conducting polymers (Chan et al., 2001). We are interested in the design of photoluminescent heterometallic cluster complexes by self-assembly between two metal components, one with alkynyl ligands and the other with vacant coordination sites. Thus, the reaction between Pt(dmbpy)(C2Ph)2, with two alkynyl ligands, and [Ag(PPh3)2(MeCN)]+, with a vacant coordination site, was expected to afford a Pt–Ag heteronuclear species. However, the product isolated from the reaction was the title compound, (I). A perspective drawing of the complex with atomic numbering scheme is depicted in Fig. 1 and selected geometric parameters are presented in Table 1.
The Pt atom is located in a distorted square-planar coordination geometry. The Pt—P distance is 2.246 (2) Å, which is slighlty shorter than that observed in the complex of PtCuCl(C2Bu)2(PMe2Ph)2 [2.300 (3) Å; Yamazaki & Deeming, 1993]. The Pt—N distances are 2.068 (6) and 2.094 (6) Å, which are similar to those observed in the complex of Pt(1,10-phenanthroline)(C9H7)2 (Hissler et al., 2000).