metal-organic compounds
Bis[bis(diphenylthiophosphinyl)amido-κ2S,S′]platinum(II)
aUniversity of Ege, Faculty of Science, Department of Chemistry, 35100 Izmir, Turkey, and bUniversity of Ondokuzmay, Faculty of Science, Department of Physics, 55139 Samsun, Turkey
*Correspondence e-mail: irislisevil@hotmail.com
In the title compound, [Pt(C24H20NP2S2)2], the Pt atom is in a distorted square-planar environment and contains two six-membered carbon-free chelate rings, one in twist-boat and the other in a half-chair conformation. Two phenyl groups are disordered over two set of sites in ratios of 0.721 (13):0.279 (13) and 0.71 (7):0.29 (7).
Related literature
For general background to imidodiphosphinedichalcogenides, see: Schmidpeter & Groger (1966); Woollins (1996); Haiduc (1997); Silvestru et al. (1998); Sekar & Ibers (2006); Crouch et al. (2003); Abbati et al. (2001). For related structures, see: Yanar et al. (2007); Bhattacharyya & Woollins (1995); İrişli & Yanar (2006); Berry et al. (1988). For geometric analysis, see: Cremer & Pople (1975)
Experimental
Crystal data
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Data collection: X-AREA (Stoe & Cie, 2002); cell X-AREA; data reduction: X-RED32 (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
Supporting information
10.1107/S1600536811010117/jj2077sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536811010117/jj2077Isup2.hkl
As reactive substances, K2PtCl4 (0,108 g; 0.24 mmol) and dppaS2 (0.1 g; 0.24 mmol) were dissolved in dichloromethane-methanol solvent system, the stirring solution was refluxed overnight and then yellow solid was collapsed, washed with pentane and recrystalized from dichloromethane/diethylether. Complex (I) was also synthesized in the literature by a different reaction pathway (Bhattacharyya & Woollins, 1995).
All H atoms were refined using a riding model with C—H = 0.93 Å and Uiso(H) = 1.2 Ueq(C). There are positional disorders in the aromatic rings attached to the P2 and P3 atoms with the sof values of 0.721 (13) (C23A, C24A), 0.279 (13) (C23B, C24B), 0.71 (7) (C34A, C35A) and 0.29 (7) (C34B, C35B).
Data collection: X-AREA (Stoe & Cie, 2002); cell
X-AREA (Stoe & Cie, 2002); data reduction: X-RED32 (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).[Pt(C24H20NP2S2)2] | Z = 2 |
Mr = 1092.03 | F(000) = 1088 |
Triclinic, P1 | Dx = 1.574 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.1103 (4) Å | Cell parameters from 23061 reflections |
b = 10.7023 (4) Å | θ = 1.7–27.3° |
c = 23.9258 (9) Å | µ = 3.40 mm−1 |
α = 98.137 (3)° | T = 296 K |
β = 90.496 (3)° | Prism, yellow |
γ = 115.563 (3)° | 0.56 × 0.32 × 0.08 mm |
V = 2304.86 (15) Å3 |
Stoe IPDS 2 diffractometer | 9495 independent reflections |
Radiation source: fine-focus sealed tube | 8823 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
rotation method scans | θmax = 26.5°, θmin = 1.7° |
Absorption correction: integration (X-RED32; Stoe & Cie, 2002) | h = −12→12 |
Tmin = 0.302, Tmax = 0.790 | k = −13→13 |
23061 measured reflections | l = −30→30 |
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) = 0.066 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.036P)2 + 1.3319P] where P = (Fo2 + 2Fc2)/3 |
9495 reflections | (Δ/σ)max = 0.002 |
570 parameters | Δρmax = 0.82 e Å−3 |
24 restraints | Δρmin = −0.79 e Å−3 |
[Pt(C24H20NP2S2)2] | γ = 115.563 (3)° |
Mr = 1092.03 | V = 2304.86 (15) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.1103 (4) Å | Mo Kα radiation |
b = 10.7023 (4) Å | µ = 3.40 mm−1 |
c = 23.9258 (9) Å | T = 296 K |
α = 98.137 (3)° | 0.56 × 0.32 × 0.08 mm |
β = 90.496 (3)° |
Stoe IPDS 2 diffractometer | 9495 independent reflections |
Absorption correction: integration (X-RED32; Stoe & Cie, 2002) | 8823 reflections with I > 2σ(I) |
Tmin = 0.302, Tmax = 0.790 | Rint = 0.033 |
23061 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 24 restraints |
wR(F2) = 0.066 | H-atom parameters constrained |
S = 1.03 | Δρmax = 0.82 e Å−3 |
9495 reflections | Δρmin = −0.79 e Å−3 |
570 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 | Occ. (<1) | |
C1 | 0.8948 (4) | 0.3729 (3) | 0.59754 (14) | 0.0444 (7) | |
C2 | 1.0207 (4) | 0.4658 (4) | 0.57643 (18) | 0.0621 (9) | |
H2 | 1.0238 | 0.5476 | 0.5661 | 0.074* | |
C3 | 1.1416 (5) | 0.4379 (6) | 0.5706 (2) | 0.0845 (14) | |
H3 | 1.2266 | 0.5017 | 0.5574 | 0.101* | |
C4 | 1.1354 (6) | 0.3154 (6) | 0.5844 (2) | 0.0906 (16) | |
H4 | 1.2162 | 0.2959 | 0.5800 | 0.109* | |
C5 | 1.0115 (6) | 0.2220 (6) | 0.6044 (2) | 0.0864 (15) | |
H5 | 1.0082 | 0.1391 | 0.6135 | 0.104* | |
C6 | 0.8916 (5) | 0.2502 (4) | 0.61133 (19) | 0.0640 (10) | |
H6 | 0.8079 | 0.1865 | 0.6253 | 0.077* | |
C7 | 0.6165 (3) | 0.3202 (3) | 0.54114 (13) | 0.0413 (6) | |
C8 | 0.6247 (6) | 0.2111 (5) | 0.50558 (19) | 0.0770 (13) | |
H8 | 0.6995 | 0.1853 | 0.5123 | 0.092* | |
C9 | 0.5221 (7) | 0.1398 (6) | 0.4599 (2) | 0.0991 (19) | |
H9 | 0.5282 | 0.0658 | 0.4363 | 0.119* | |
C10 | 0.4126 (5) | 0.1765 (4) | 0.44895 (18) | 0.0720 (12) | |
H10 | 0.3434 | 0.1274 | 0.4184 | 0.086* | |
C11 | 0.4052 (4) | 0.2855 (4) | 0.48304 (17) | 0.0629 (10) | |
H11 | 0.3317 | 0.3123 | 0.4753 | 0.076* | |
C12 | 0.5062 (4) | 0.3570 (4) | 0.52921 (15) | 0.0528 (8) | |
H12 | 0.4992 | 0.4310 | 0.5525 | 0.063* | |
C13 | 0.3674 (4) | 0.1330 (4) | 0.87188 (16) | 0.0552 (8) | |
C14 | 0.3001 (5) | 0.0020 (5) | 0.8382 (2) | 0.0762 (13) | |
H14 | 0.3096 | −0.0051 | 0.7994 | 0.091* | |
C15 | 0.2197 (6) | −0.1179 (5) | 0.8606 (3) | 0.0896 (15) | |
H15 | 0.1756 | −0.2050 | 0.8375 | 0.108* | |
C16 | 0.2062 (6) | −0.1063 (6) | 0.9175 (3) | 0.0957 (17) | |
H16 | 0.1498 | −0.1861 | 0.9329 | 0.115* | |
C17 | 0.2725 (8) | 0.0178 (7) | 0.9516 (3) | 0.110 (2) | |
H17 | 0.2637 | 0.0226 | 0.9904 | 0.132* | |
C18 | 0.3546 (7) | 0.1400 (5) | 0.9293 (2) | 0.0876 (15) | |
H18 | 0.4004 | 0.2258 | 0.9533 | 0.105* | |
C19 | 0.3316 (4) | 0.3238 (4) | 0.80632 (16) | 0.0580 (9) | |
C20 | 0.1798 (6) | 0.2294 (6) | 0.8039 (3) | 0.1047 (19) | |
H20 | 0.1489 | 0.1464 | 0.8188 | 0.126* | |
C21 | 0.0774 (7) | 0.2653 (8) | 0.7783 (3) | 0.120 (2) | |
H21 | −0.0224 | 0.2049 | 0.7758 | 0.144* | |
C22 | 0.1238 (7) | 0.3876 (7) | 0.7573 (3) | 0.0986 (17) | |
H22 | 0.0576 | 0.4057 | 0.7366 | 0.118* | |
C23A | 0.2620 (12) | 0.4801 (12) | 0.7664 (6) | 0.120 (4) | 0.721 (13) |
H23A | 0.2900 | 0.5707 | 0.7589 | 0.144* | 0.721 (13) |
C24A | 0.3672 (9) | 0.4430 (10) | 0.7871 (5) | 0.097 (3) | 0.721 (13) |
H24A | 0.4661 | 0.5046 | 0.7874 | 0.116* | 0.721 (13) |
C23B | 0.245 (2) | 0.397 (3) | 0.7331 (9) | 0.081 (6) | 0.279 (13) |
H23B | 0.2656 | 0.4355 | 0.7000 | 0.097* | 0.279 (13) |
C24B | 0.343 (2) | 0.352 (3) | 0.7540 (10) | 0.089 (6) | 0.279 (13) |
H24B | 0.4141 | 0.3421 | 0.7319 | 0.107* | 0.279 (13) |
C25 | 0.7966 (4) | 0.5871 (4) | 0.96474 (15) | 0.0586 (9) | |
C26 | 0.7835 (8) | 0.4771 (6) | 0.9929 (2) | 0.107 (2) | |
H26 | 0.7258 | 0.3844 | 0.9765 | 0.128* | |
C27 | 0.8574 (12) | 0.5080 (10) | 1.0455 (3) | 0.156 (4) | |
H27 | 0.8484 | 0.4352 | 1.0646 | 0.187* | |
C28 | 0.9427 (9) | 0.6421 (10) | 1.0699 (2) | 0.127 (3) | |
H28 | 0.9911 | 0.6606 | 1.1055 | 0.152* | |
C29 | 0.9579 (7) | 0.7498 (7) | 1.0424 (2) | 0.1047 (19) | |
H29 | 1.0184 | 0.8418 | 1.0588 | 0.126* | |
C30 | 0.8831 (5) | 0.7222 (5) | 0.99010 (19) | 0.0776 (12) | |
H30 | 0.8916 | 0.7962 | 0.9719 | 0.093* | |
C31 | 0.6861 (5) | 0.6984 (4) | 0.88311 (17) | 0.0619 (9) | |
C32 | 0.5663 (7) | 0.7108 (7) | 0.9052 (3) | 0.111 (2) | |
H32 | 0.4996 | 0.6419 | 0.9238 | 0.133* | |
C33 | 0.5481 (11) | 0.8326 (10) | 0.8989 (4) | 0.148 (3) | |
H33 | 0.4668 | 0.8403 | 0.9138 | 0.178* | |
C34A | 0.629 (4) | 0.926 (2) | 0.8758 (11) | 0.112 (8) | 0.71 (7) |
H34A | 0.6132 | 1.0050 | 0.8749 | 0.135* | 0.71 (7) |
C35A | 0.743 (4) | 0.914 (2) | 0.8511 (7) | 0.086 (6) | 0.71 (7) |
H35A | 0.7993 | 0.9813 | 0.8298 | 0.103* | 0.71 (7) |
C34B | 0.677 (5) | 0.944 (5) | 0.860 (2) | 0.084 (11) | 0.29 (7) |
H34B | 0.6607 | 1.0144 | 0.8473 | 0.101* | 0.29 (7) |
C35B | 0.804 (6) | 0.932 (4) | 0.8483 (17) | 0.071 (8) | 0.29 (7) |
H35B | 0.8893 | 0.9999 | 0.8370 | 0.085* | 0.29 (7) |
C36 | 0.7814 (6) | 0.8013 (5) | 0.8561 (2) | 0.0790 (13) | |
H36 | 0.8657 | 0.7989 | 0.8418 | 0.095* | |
C37 | 0.7337 (4) | 0.7682 (3) | 0.67965 (14) | 0.0489 (7) | |
C38 | 0.5841 (5) | 0.6851 (5) | 0.6757 (2) | 0.0793 (13) | |
H38 | 0.5474 | 0.5885 | 0.6648 | 0.095* | |
C39 | 0.4883 (6) | 0.7448 (6) | 0.6880 (3) | 0.1044 (19) | |
H39 | 0.3875 | 0.6880 | 0.6845 | 0.125* | |
C40 | 0.5400 (7) | 0.8856 (6) | 0.7053 (2) | 0.0897 (15) | |
H40 | 0.4752 | 0.9244 | 0.7150 | 0.108* | |
C41 | 0.6860 (6) | 0.9683 (5) | 0.70833 (19) | 0.0745 (12) | |
H41 | 0.7211 | 1.0648 | 0.7190 | 0.089* | |
C42 | 0.7838 (5) | 0.9124 (4) | 0.69590 (17) | 0.0609 (9) | |
H42 | 0.8841 | 0.9712 | 0.6984 | 0.073* | |
C43 | 1.0174 (4) | 0.8296 (3) | 0.63714 (14) | 0.0448 (7) | |
C44 | 1.1319 (4) | 0.9254 (4) | 0.67540 (18) | 0.0662 (11) | |
H44 | 1.1286 | 0.9183 | 0.7137 | 0.079* | |
C45 | 1.2513 (5) | 1.0315 (5) | 0.6567 (2) | 0.0773 (13) | |
H45 | 1.3279 | 1.0958 | 0.6825 | 0.093* | |
C46 | 1.2566 (4) | 1.0421 (4) | 0.6001 (2) | 0.0654 (10) | |
H46 | 1.3376 | 1.1123 | 0.5875 | 0.078* | |
C47 | 1.1428 (4) | 0.9494 (4) | 0.56251 (18) | 0.0608 (9) | |
H47 | 1.1460 | 0.9579 | 0.5243 | 0.073* | |
C48 | 1.0225 (4) | 0.8429 (3) | 0.58052 (15) | 0.0507 (8) | |
H48 | 0.9453 | 0.7805 | 0.5546 | 0.061* | |
N1 | 0.7810 (3) | 0.5722 (2) | 0.60647 (11) | 0.0416 (5) | |
N2 | 0.5590 (3) | 0.4148 (3) | 0.89129 (13) | 0.0562 (7) | |
P1 | 0.73768 (8) | 0.41014 (7) | 0.60417 (3) | 0.03652 (15) | |
P2 | 0.46930 (10) | 0.28923 (9) | 0.84166 (4) | 0.04727 (18) | |
P3 | 0.71250 (10) | 0.54698 (9) | 0.89377 (4) | 0.04749 (19) | |
P4 | 0.85814 (8) | 0.69144 (7) | 0.66001 (3) | 0.03865 (16) | |
S1 | 0.61827 (9) | 0.31817 (8) | 0.66701 (3) | 0.04800 (18) | |
S2 | 0.58863 (10) | 0.23147 (8) | 0.78461 (4) | 0.04756 (18) | |
S3 | 0.86728 (9) | 0.52805 (9) | 0.84426 (3) | 0.04726 (17) | |
S4 | 0.93207 (9) | 0.63793 (8) | 0.72772 (4) | 0.04849 (18) | |
Pt1 | 0.746243 (12) | 0.437756 (11) | 0.754094 (4) | 0.03693 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0485 (17) | 0.0486 (16) | 0.0385 (16) | 0.0237 (14) | 0.0012 (13) | 0.0065 (12) |
C2 | 0.060 (2) | 0.065 (2) | 0.071 (3) | 0.0325 (18) | 0.0171 (19) | 0.0230 (19) |
C3 | 0.063 (3) | 0.100 (3) | 0.106 (4) | 0.043 (2) | 0.035 (3) | 0.037 (3) |
C4 | 0.086 (3) | 0.123 (4) | 0.105 (4) | 0.077 (3) | 0.030 (3) | 0.040 (3) |
C5 | 0.101 (4) | 0.097 (3) | 0.103 (4) | 0.074 (3) | 0.027 (3) | 0.042 (3) |
C6 | 0.070 (2) | 0.063 (2) | 0.074 (3) | 0.0389 (19) | 0.012 (2) | 0.0246 (19) |
C7 | 0.0464 (16) | 0.0417 (14) | 0.0327 (15) | 0.0168 (12) | 0.0003 (12) | 0.0048 (11) |
C8 | 0.095 (3) | 0.085 (3) | 0.062 (3) | 0.062 (3) | −0.027 (2) | −0.026 (2) |
C9 | 0.139 (5) | 0.099 (3) | 0.066 (3) | 0.076 (4) | −0.047 (3) | −0.042 (3) |
C10 | 0.085 (3) | 0.067 (2) | 0.049 (2) | 0.025 (2) | −0.025 (2) | −0.0065 (18) |
C11 | 0.056 (2) | 0.072 (2) | 0.057 (2) | 0.0264 (18) | −0.0150 (17) | 0.0070 (18) |
C12 | 0.0517 (19) | 0.0537 (18) | 0.051 (2) | 0.0236 (15) | −0.0061 (15) | −0.0009 (14) |
C13 | 0.0458 (18) | 0.069 (2) | 0.051 (2) | 0.0222 (16) | 0.0090 (15) | 0.0204 (16) |
C14 | 0.065 (3) | 0.071 (3) | 0.065 (3) | 0.002 (2) | 0.000 (2) | 0.017 (2) |
C15 | 0.072 (3) | 0.072 (3) | 0.103 (4) | 0.007 (2) | 0.007 (3) | 0.027 (3) |
C16 | 0.094 (4) | 0.088 (3) | 0.114 (5) | 0.037 (3) | 0.041 (3) | 0.055 (3) |
C17 | 0.143 (6) | 0.111 (4) | 0.074 (4) | 0.045 (4) | 0.048 (4) | 0.044 (3) |
C18 | 0.118 (4) | 0.079 (3) | 0.057 (3) | 0.032 (3) | 0.027 (3) | 0.019 (2) |
C19 | 0.061 (2) | 0.075 (2) | 0.0450 (19) | 0.0366 (19) | 0.0041 (16) | 0.0087 (16) |
C20 | 0.073 (3) | 0.102 (4) | 0.139 (6) | 0.037 (3) | −0.008 (3) | 0.025 (4) |
C21 | 0.076 (4) | 0.144 (6) | 0.141 (6) | 0.053 (4) | −0.022 (4) | 0.008 (5) |
C22 | 0.100 (4) | 0.131 (5) | 0.098 (4) | 0.076 (4) | 0.000 (3) | 0.036 (4) |
C23A | 0.115 (6) | 0.101 (6) | 0.149 (8) | 0.046 (5) | −0.024 (5) | 0.042 (6) |
C24A | 0.074 (4) | 0.097 (5) | 0.123 (7) | 0.030 (4) | −0.010 (4) | 0.056 (5) |
C23B | 0.075 (8) | 0.108 (10) | 0.071 (9) | 0.042 (7) | 0.003 (6) | 0.039 (7) |
C24B | 0.072 (8) | 0.120 (11) | 0.079 (9) | 0.044 (7) | 0.010 (7) | 0.025 (8) |
C25 | 0.067 (2) | 0.081 (2) | 0.0344 (17) | 0.040 (2) | 0.0002 (15) | 0.0023 (16) |
C26 | 0.160 (6) | 0.098 (4) | 0.068 (3) | 0.063 (4) | −0.028 (4) | 0.013 (3) |
C27 | 0.262 (11) | 0.173 (7) | 0.070 (4) | 0.132 (8) | −0.045 (6) | 0.018 (5) |
C28 | 0.169 (7) | 0.193 (8) | 0.049 (3) | 0.118 (6) | −0.033 (4) | −0.011 (4) |
C29 | 0.110 (4) | 0.132 (5) | 0.057 (3) | 0.051 (4) | −0.025 (3) | −0.022 (3) |
C30 | 0.084 (3) | 0.090 (3) | 0.050 (2) | 0.033 (2) | −0.012 (2) | 0.001 (2) |
C31 | 0.074 (3) | 0.065 (2) | 0.052 (2) | 0.039 (2) | −0.0100 (18) | −0.0012 (17) |
C32 | 0.109 (5) | 0.112 (4) | 0.146 (6) | 0.078 (4) | 0.022 (4) | 0.024 (4) |
C33 | 0.156 (8) | 0.155 (7) | 0.192 (10) | 0.128 (7) | 0.005 (7) | 0.011 (7) |
C34A | 0.18 (2) | 0.097 (10) | 0.099 (11) | 0.098 (13) | −0.006 (12) | 0.008 (7) |
C35A | 0.110 (18) | 0.078 (7) | 0.086 (6) | 0.053 (9) | −0.011 (10) | 0.022 (5) |
C34B | 0.08 (2) | 0.11 (2) | 0.08 (2) | 0.064 (15) | −0.004 (14) | 0.034 (16) |
C35B | 0.063 (16) | 0.073 (13) | 0.076 (13) | 0.036 (12) | −0.015 (12) | −0.012 (11) |
C36 | 0.110 (4) | 0.065 (2) | 0.064 (3) | 0.043 (3) | −0.011 (3) | 0.003 (2) |
C37 | 0.0583 (19) | 0.0487 (16) | 0.0424 (17) | 0.0267 (15) | 0.0042 (14) | 0.0050 (13) |
C38 | 0.059 (2) | 0.066 (2) | 0.115 (4) | 0.030 (2) | 0.027 (3) | 0.013 (2) |
C39 | 0.072 (3) | 0.110 (4) | 0.141 (6) | 0.051 (3) | 0.032 (3) | 0.012 (4) |
C40 | 0.102 (4) | 0.100 (4) | 0.094 (4) | 0.073 (3) | 0.024 (3) | 0.004 (3) |
C41 | 0.109 (4) | 0.070 (2) | 0.063 (3) | 0.059 (3) | 0.010 (2) | 0.0019 (19) |
C42 | 0.078 (3) | 0.0532 (19) | 0.053 (2) | 0.0322 (18) | 0.0022 (18) | 0.0003 (15) |
C43 | 0.0452 (16) | 0.0393 (14) | 0.0475 (18) | 0.0158 (13) | −0.0006 (13) | 0.0087 (12) |
C44 | 0.059 (2) | 0.061 (2) | 0.055 (2) | 0.0025 (17) | −0.0084 (18) | 0.0166 (17) |
C45 | 0.055 (2) | 0.063 (2) | 0.084 (3) | −0.0038 (18) | −0.011 (2) | 0.020 (2) |
C46 | 0.050 (2) | 0.0533 (19) | 0.088 (3) | 0.0124 (16) | 0.016 (2) | 0.028 (2) |
C47 | 0.065 (2) | 0.061 (2) | 0.058 (2) | 0.0255 (18) | 0.0190 (19) | 0.0211 (17) |
C48 | 0.0528 (19) | 0.0471 (16) | 0.0490 (19) | 0.0187 (14) | 0.0042 (15) | 0.0081 (14) |
N1 | 0.0472 (14) | 0.0375 (12) | 0.0385 (13) | 0.0175 (11) | −0.0024 (11) | 0.0047 (10) |
N2 | 0.0543 (17) | 0.0666 (18) | 0.0423 (16) | 0.0235 (14) | 0.0109 (13) | 0.0018 (13) |
P1 | 0.0385 (4) | 0.0349 (3) | 0.0330 (4) | 0.0137 (3) | 0.0002 (3) | 0.0037 (3) |
P2 | 0.0481 (4) | 0.0570 (5) | 0.0376 (4) | 0.0233 (4) | 0.0071 (3) | 0.0093 (3) |
P3 | 0.0529 (5) | 0.0554 (5) | 0.0359 (4) | 0.0266 (4) | −0.0018 (3) | 0.0030 (3) |
P4 | 0.0409 (4) | 0.0348 (3) | 0.0366 (4) | 0.0134 (3) | −0.0001 (3) | 0.0051 (3) |
S1 | 0.0479 (4) | 0.0441 (4) | 0.0349 (4) | 0.0051 (3) | 0.0033 (3) | 0.0037 (3) |
S2 | 0.0552 (5) | 0.0414 (4) | 0.0464 (4) | 0.0202 (3) | 0.0145 (4) | 0.0108 (3) |
S3 | 0.0453 (4) | 0.0600 (4) | 0.0358 (4) | 0.0225 (4) | −0.0016 (3) | 0.0076 (3) |
S4 | 0.0466 (4) | 0.0460 (4) | 0.0425 (4) | 0.0090 (3) | −0.0066 (3) | 0.0132 (3) |
Pt1 | 0.04044 (7) | 0.03858 (6) | 0.03214 (7) | 0.01761 (5) | 0.00324 (4) | 0.00568 (4) |
C1—C6 | 1.386 (5) | C27—H27 | 0.9300 |
C1—C2 | 1.388 (5) | C28—C29 | 1.359 (10) |
C1—P1 | 1.800 (3) | C28—H28 | 0.9300 |
C2—C3 | 1.381 (6) | C29—C30 | 1.384 (7) |
C2—H2 | 0.9300 | C29—H29 | 0.9300 |
C3—C4 | 1.372 (7) | C30—H30 | 0.9300 |
C3—H3 | 0.9300 | C31—C36 | 1.362 (7) |
C4—C5 | 1.365 (7) | C31—C32 | 1.377 (7) |
C4—H4 | 0.9300 | C31—P3 | 1.803 (4) |
C5—C6 | 1.375 (6) | C32—C33 | 1.421 (9) |
C5—H5 | 0.9300 | C32—H32 | 0.9300 |
C6—H6 | 0.9300 | C33—C34A | 1.19 (4) |
C7—C12 | 1.373 (5) | C33—C34B | 1.72 (6) |
C7—C8 | 1.378 (5) | C33—H33 | 0.9300 |
C7—P1 | 1.800 (3) | C34A—C35A | 1.35 (2) |
C8—C9 | 1.384 (6) | C34A—H34A | 0.9300 |
C8—H8 | 0.9300 | C35A—C36 | 1.432 (18) |
C9—C10 | 1.360 (7) | C35A—H35A | 0.9300 |
C9—H9 | 0.9300 | C34B—C35B | 1.37 (4) |
C10—C11 | 1.355 (6) | C34B—H34B | 0.9300 |
C10—H10 | 0.9300 | C35B—C36 | 1.35 (4) |
C11—C12 | 1.384 (5) | C35B—H35B | 0.9300 |
C11—H11 | 0.9300 | C36—H36 | 0.9300 |
C12—H12 | 0.9300 | C37—C38 | 1.379 (6) |
C13—C18 | 1.376 (6) | C37—C42 | 1.393 (5) |
C13—C14 | 1.388 (6) | C37—P4 | 1.809 (3) |
C13—P2 | 1.802 (4) | C38—C39 | 1.385 (6) |
C14—C15 | 1.378 (6) | C38—H38 | 0.9300 |
C14—H14 | 0.9300 | C39—C40 | 1.363 (7) |
C15—C16 | 1.361 (8) | C39—H39 | 0.9300 |
C15—H15 | 0.9300 | C40—C41 | 1.349 (7) |
C16—C17 | 1.340 (8) | C40—H40 | 0.9300 |
C16—H16 | 0.9300 | C41—C42 | 1.375 (6) |
C17—C18 | 1.397 (7) | C41—H41 | 0.9300 |
C17—H17 | 0.9300 | C42—H42 | 0.9300 |
C18—H18 | 0.9300 | C43—C48 | 1.381 (5) |
C19—C24A | 1.319 (8) | C43—C44 | 1.386 (5) |
C19—C24B | 1.32 (2) | C43—P4 | 1.808 (3) |
C19—C20 | 1.422 (7) | C44—C45 | 1.384 (5) |
C19—P2 | 1.817 (4) | C44—H44 | 0.9300 |
C20—C21 | 1.412 (8) | C45—C46 | 1.375 (6) |
C20—H20 | 0.9300 | C45—H45 | 0.9300 |
C21—C22 | 1.359 (9) | C46—C47 | 1.365 (6) |
C21—H21 | 0.9300 | C46—H46 | 0.9300 |
C22—C23A | 1.312 (11) | C47—C48 | 1.384 (5) |
C22—C23B | 1.33 (2) | C47—H47 | 0.9300 |
C22—H22 | 0.9300 | C48—H48 | 0.9300 |
C23A—C24A | 1.395 (12) | N1—P1 | 1.588 (2) |
C23A—H23A | 0.9300 | N1—P4 | 1.593 (3) |
C24A—H24A | 0.9300 | N2—P3 | 1.579 (3) |
C23B—C24B | 1.39 (3) | N2—P2 | 1.586 (3) |
C23B—H23B | 0.9300 | P1—S1 | 2.0278 (11) |
C24B—H24B | 0.9300 | P2—S2 | 2.0333 (12) |
C25—C30 | 1.369 (6) | P3—S3 | 2.0325 (12) |
C25—C26 | 1.396 (6) | P4—S4 | 2.0304 (11) |
C25—P3 | 1.801 (4) | S1—Pt1 | 2.3286 (8) |
C26—C27 | 1.381 (8) | S2—Pt1 | 2.3209 (8) |
C26—H26 | 0.9300 | S3—Pt1 | 2.3299 (8) |
C27—C28 | 1.352 (11) | S4—Pt1 | 2.3339 (8) |
C6—C1—C2 | 118.6 (3) | C29—C30—H30 | 119.6 |
C6—C1—P1 | 121.4 (3) | C36—C31—C32 | 119.5 (5) |
C2—C1—P1 | 119.9 (3) | C36—C31—P3 | 122.9 (4) |
C3—C2—C1 | 120.6 (4) | C32—C31—P3 | 117.5 (4) |
C3—C2—H2 | 119.7 | C31—C32—C33 | 117.8 (7) |
C1—C2—H2 | 119.7 | C31—C32—H32 | 121.1 |
C4—C3—C2 | 119.6 (4) | C33—C32—H32 | 121.1 |
C4—C3—H3 | 120.2 | C34A—C33—C32 | 125.2 (15) |
C2—C3—H3 | 120.2 | C32—C33—C34B | 114.4 (18) |
C5—C4—C3 | 120.5 (4) | C34A—C33—H33 | 117.4 |
C5—C4—H4 | 119.8 | C32—C33—H33 | 117.4 |
C3—C4—H4 | 119.8 | C34B—C33—H33 | 128.1 |
C4—C5—C6 | 120.3 (4) | C33—C34A—C35A | 118.6 (15) |
C4—C5—H5 | 119.9 | C33—C34A—H34A | 120.7 |
C6—C5—H5 | 119.9 | C35A—C34A—H34A | 120.7 |
C5—C6—C1 | 120.4 (4) | C34A—C35A—C36 | 123.2 (15) |
C5—C6—H6 | 119.8 | C34A—C35A—H35A | 118.4 |
C1—C6—H6 | 119.8 | C36—C35A—H35A | 118.4 |
C12—C7—C8 | 118.2 (3) | C35B—C34B—C33 | 122 (3) |
C12—C7—P1 | 118.8 (2) | C35B—C34B—H34B | 119.2 |
C8—C7—P1 | 122.9 (3) | C33—C34B—H34B | 119.2 |
C7—C8—C9 | 120.2 (4) | C36—C35B—C34B | 107 (4) |
C7—C8—H8 | 119.9 | C36—C35B—H35B | 126.6 |
C9—C8—H8 | 119.9 | C34B—C35B—H35B | 126.6 |
C10—C9—C8 | 120.8 (4) | C35B—C36—C31 | 137 (2) |
C10—C9—H9 | 119.6 | C31—C36—C35A | 115.4 (16) |
C8—C9—H9 | 119.6 | C35B—C36—H36 | 100.0 |
C11—C10—C9 | 119.4 (4) | C31—C36—H36 | 122.3 |
C11—C10—H10 | 120.3 | C35A—C36—H36 | 122.3 |
C9—C10—H10 | 120.3 | C38—C37—C42 | 117.9 (4) |
C10—C11—C12 | 120.5 (4) | C38—C37—P4 | 120.2 (3) |
C10—C11—H11 | 119.8 | C42—C37—P4 | 121.7 (3) |
C12—C11—H11 | 119.8 | C37—C38—C39 | 120.3 (4) |
C7—C12—C11 | 120.9 (3) | C37—C38—H38 | 119.9 |
C7—C12—H12 | 119.6 | C39—C38—H38 | 119.9 |
C11—C12—H12 | 119.6 | C40—C39—C38 | 120.8 (5) |
C18—C13—C14 | 117.8 (4) | C40—C39—H39 | 119.6 |
C18—C13—P2 | 120.9 (3) | C38—C39—H39 | 119.6 |
C14—C13—P2 | 121.3 (3) | C41—C40—C39 | 119.4 (4) |
C15—C14—C13 | 121.9 (5) | C41—C40—H40 | 120.3 |
C15—C14—H14 | 119.0 | C39—C40—H40 | 120.3 |
C13—C14—H14 | 119.0 | C40—C41—C42 | 121.2 (4) |
C16—C15—C14 | 118.5 (5) | C40—C41—H41 | 119.4 |
C16—C15—H15 | 120.7 | C42—C41—H41 | 119.4 |
C14—C15—H15 | 120.7 | C41—C42—C37 | 120.4 (4) |
C17—C16—C15 | 121.4 (5) | C41—C42—H42 | 119.8 |
C17—C16—H16 | 119.3 | C37—C42—H42 | 119.8 |
C15—C16—H16 | 119.3 | C48—C43—C44 | 119.3 (3) |
C16—C17—C18 | 120.4 (5) | C48—C43—P4 | 119.2 (2) |
C16—C17—H17 | 119.8 | C44—C43—P4 | 121.5 (3) |
C18—C17—H17 | 119.8 | C45—C44—C43 | 120.2 (4) |
C13—C18—C17 | 119.8 (5) | C45—C44—H44 | 119.9 |
C13—C18—H18 | 120.1 | C43—C44—H44 | 119.9 |
C17—C18—H18 | 120.1 | C46—C45—C44 | 120.0 (4) |
C24A—C19—C24B | 49.2 (10) | C46—C45—H45 | 120.0 |
C24A—C19—C20 | 117.7 (5) | C44—C45—H45 | 120.0 |
C24B—C19—C20 | 100.7 (10) | C47—C46—C45 | 119.9 (3) |
C24A—C19—P2 | 121.2 (4) | C47—C46—H46 | 120.1 |
C24B—C19—P2 | 121.7 (9) | C45—C46—H46 | 120.1 |
C20—C19—P2 | 120.7 (4) | C46—C47—C48 | 120.8 (4) |
C21—C20—C19 | 118.1 (6) | C46—C47—H47 | 119.6 |
C21—C20—H20 | 120.9 | C48—C47—H47 | 119.6 |
C19—C20—H20 | 120.9 | C43—C48—C47 | 119.8 (3) |
C22—C21—C20 | 120.4 (6) | C43—C48—H48 | 120.1 |
C22—C21—H21 | 119.8 | C47—C48—H48 | 120.1 |
C20—C21—H21 | 119.8 | P1—N1—P4 | 125.54 (17) |
C23A—C22—C23B | 47.3 (10) | P3—N2—P2 | 131.51 (19) |
C23A—C22—C21 | 119.9 (6) | N1—P1—C1 | 112.15 (15) |
C23B—C22—C21 | 102.8 (10) | N1—P1—C7 | 106.37 (14) |
C23A—C22—H22 | 120.1 | C1—P1—C7 | 107.27 (15) |
C23B—C22—H22 | 117.1 | N1—P1—S1 | 116.37 (11) |
C21—C22—H22 | 120.1 | C1—P1—S1 | 110.13 (11) |
C22—C23A—C24A | 120.2 (8) | C7—P1—S1 | 103.75 (10) |
C22—C23A—H23A | 119.9 | N2—P2—C13 | 108.81 (18) |
C24A—C23A—H23A | 119.9 | N2—P2—C19 | 110.03 (18) |
C19—C24A—C23A | 122.5 (8) | C13—P2—C19 | 105.46 (18) |
C19—C24A—H24A | 118.7 | N2—P2—S2 | 116.77 (12) |
C23A—C24A—H24A | 118.7 | C13—P2—S2 | 103.90 (13) |
C22—C23B—C24B | 124.3 (16) | C19—P2—S2 | 111.06 (13) |
C22—C23B—H23B | 117.8 | N2—P3—C25 | 107.48 (18) |
C24B—C23B—H23B | 117.8 | N2—P3—C31 | 110.2 (2) |
C19—C24B—C23B | 117.9 (17) | C25—P3—C31 | 105.70 (19) |
C19—C24B—H24B | 121.0 | N2—P3—S3 | 117.98 (12) |
C23B—C24B—H24B | 121.0 | C25—P3—S3 | 103.84 (13) |
C30—C25—C26 | 118.9 (4) | C31—P3—S3 | 110.71 (15) |
C30—C25—P3 | 121.8 (3) | N1—P4—C43 | 107.67 (15) |
C26—C25—P3 | 119.1 (4) | N1—P4—C37 | 107.40 (15) |
C27—C26—C25 | 119.0 (6) | C43—P4—C37 | 105.66 (15) |
C27—C26—H26 | 120.5 | N1—P4—S4 | 117.64 (10) |
C25—C26—H26 | 120.5 | C43—P4—S4 | 105.99 (11) |
C28—C27—C26 | 121.3 (7) | C37—P4—S4 | 111.77 (12) |
C28—C27—H27 | 119.3 | P1—S1—Pt1 | 109.16 (4) |
C26—C27—H27 | 119.3 | P2—S2—Pt1 | 104.97 (4) |
C27—C28—C29 | 120.2 (6) | P3—S3—Pt1 | 104.36 (4) |
C27—C28—H28 | 119.9 | P4—S4—Pt1 | 110.20 (4) |
C29—C28—H28 | 119.9 | S2—Pt1—S1 | 82.41 (3) |
C28—C29—C30 | 119.8 (6) | S2—Pt1—S3 | 90.87 (3) |
C28—C29—H29 | 120.1 | S1—Pt1—S3 | 172.36 (3) |
C30—C29—H29 | 120.1 | S2—Pt1—S4 | 171.73 (3) |
C25—C30—C29 | 120.8 (5) | S1—Pt1—S4 | 101.46 (3) |
C25—C30—H30 | 119.6 | S3—Pt1—S4 | 84.75 (3) |
C6—C1—C2—C3 | −1.5 (6) | P4—N1—P1—C1 | −76.6 (2) |
P1—C1—C2—C3 | −179.4 (4) | P4—N1—P1—C7 | 166.4 (2) |
C1—C2—C3—C4 | 1.7 (8) | P4—N1—P1—S1 | 51.4 (2) |
C2—C3—C4—C5 | −0.8 (9) | C6—C1—P1—N1 | 160.7 (3) |
C3—C4—C5—C6 | −0.3 (9) | C2—C1—P1—N1 | −21.5 (3) |
C4—C5—C6—C1 | 0.6 (8) | C6—C1—P1—C7 | −82.9 (3) |
C2—C1—C6—C5 | 0.3 (7) | C2—C1—P1—C7 | 94.9 (3) |
P1—C1—C6—C5 | 178.2 (4) | C6—C1—P1—S1 | 29.4 (3) |
C12—C7—C8—C9 | −1.2 (7) | C2—C1—P1—S1 | −152.8 (3) |
P1—C7—C8—C9 | 175.6 (4) | C12—C7—P1—N1 | −44.6 (3) |
C7—C8—C9—C10 | 0.5 (9) | C8—C7—P1—N1 | 138.6 (4) |
C8—C9—C10—C11 | 0.7 (9) | C12—C7—P1—C1 | −164.8 (3) |
C9—C10—C11—C12 | −1.3 (7) | C8—C7—P1—C1 | 18.4 (4) |
C8—C7—C12—C11 | 0.6 (6) | C12—C7—P1—S1 | 78.6 (3) |
P1—C7—C12—C11 | −176.3 (3) | C8—C7—P1—S1 | −98.1 (4) |
C10—C11—C12—C7 | 0.6 (6) | P3—N2—P2—C13 | 147.7 (3) |
C18—C13—C14—C15 | 1.5 (7) | P3—N2—P2—C19 | −97.2 (3) |
P2—C13—C14—C15 | −178.8 (4) | P3—N2—P2—S2 | 30.5 (3) |
C13—C14—C15—C16 | 0.2 (8) | C18—C13—P2—N2 | 11.3 (4) |
C14—C15—C16—C17 | −1.9 (10) | C14—C13—P2—N2 | −168.3 (4) |
C15—C16—C17—C18 | 1.7 (11) | C18—C13—P2—C19 | −106.7 (4) |
C14—C13—C18—C17 | −1.7 (8) | C14—C13—P2—C19 | 73.7 (4) |
P2—C13—C18—C17 | 178.7 (5) | C18—C13—P2—S2 | 136.4 (4) |
C16—C17—C18—C13 | 0.1 (10) | C14—C13—P2—S2 | −43.2 (4) |
C24A—C19—C20—C21 | 3.5 (10) | C24A—C19—P2—N2 | 52.1 (7) |
C24B—C19—C20—C21 | −45.8 (13) | C24B—C19—P2—N2 | 110.5 (14) |
P2—C19—C20—C21 | 177.0 (5) | C20—C19—P2—N2 | −121.1 (4) |
C19—C20—C21—C22 | −0.8 (11) | C24A—C19—P2—C13 | 169.3 (7) |
C20—C21—C22—C23A | −7.6 (14) | C24B—C19—P2—C13 | −132.3 (14) |
C20—C21—C22—C23B | 40.2 (14) | C20—C19—P2—C13 | −3.9 (5) |
C23B—C22—C23A—C24A | −66.5 (14) | C24A—C19—P2—S2 | −78.7 (7) |
C21—C22—C23A—C24A | 13.0 (17) | C24B—C19—P2—S2 | −20.3 (14) |
C24B—C19—C24A—C23A | 81.6 (15) | C20—C19—P2—S2 | 108.1 (4) |
C20—C19—C24A—C23A | 1.8 (14) | P2—N2—P3—C25 | −147.3 (3) |
P2—C19—C24A—C23A | −171.7 (9) | P2—N2—P3—C31 | 98.0 (3) |
C22—C23A—C24A—C19 | −10.3 (18) | P2—N2—P3—S3 | −30.5 (3) |
C23A—C22—C23B—C24B | 84 (2) | C30—C25—P3—N2 | −145.9 (4) |
C21—C22—C23B—C24B | −35 (3) | C26—C25—P3—N2 | 39.5 (5) |
C24A—C19—C24B—C23B | −65 (2) | C30—C25—P3—C31 | −28.3 (4) |
C20—C19—C24B—C23B | 52 (2) | C26—C25—P3—C31 | 157.1 (4) |
P2—C19—C24B—C23B | −171.0 (15) | C30—C25—P3—S3 | 88.3 (4) |
C22—C23B—C24B—C19 | −14 (3) | C26—C25—P3—S3 | −86.3 (4) |
C30—C25—C26—C27 | 0.3 (10) | C36—C31—P3—N2 | −146.5 (4) |
P3—C25—C26—C27 | 175.1 (6) | C32—C31—P3—N2 | 35.7 (5) |
C25—C26—C27—C28 | −0.5 (13) | C36—C31—P3—C25 | 97.6 (4) |
C26—C27—C28—C29 | −0.4 (14) | C32—C31—P3—C25 | −80.2 (5) |
C27—C28—C29—C30 | 1.5 (12) | C36—C31—P3—S3 | −14.2 (4) |
C26—C25—C30—C29 | 0.8 (8) | C32—C31—P3—S3 | 168.0 (4) |
P3—C25—C30—C29 | −173.8 (4) | P1—N1—P4—C43 | 128.1 (2) |
C28—C29—C30—C25 | −1.8 (9) | P1—N1—P4—C37 | −118.5 (2) |
C36—C31—C32—C33 | −0.2 (9) | P1—N1—P4—S4 | 8.5 (2) |
P3—C31—C32—C33 | 177.7 (6) | C48—C43—P4—N1 | 22.8 (3) |
C31—C32—C33—C34A | −0.1 (17) | C44—C43—P4—N1 | −159.5 (3) |
C31—C32—C33—C34B | 3 (2) | C48—C43—P4—C37 | −91.7 (3) |
C32—C33—C34A—C35A | 4 (3) | C44—C43—P4—C37 | 85.9 (3) |
C34B—C33—C34A—C35A | −12 (10) | C48—C43—P4—S4 | 149.5 (2) |
C33—C34A—C35A—C36 | −7 (3) | C44—C43—P4—S4 | −32.8 (3) |
C34A—C33—C34B—C35B | 152 (15) | C38—C37—P4—N1 | 37.4 (4) |
C32—C33—C34B—C35B | −14 (5) | C42—C37—P4—N1 | −138.9 (3) |
C33—C34B—C35B—C36 | 18 (6) | C38—C37—P4—C43 | 152.1 (4) |
C34B—C35B—C36—C31 | −18 (5) | C42—C37—P4—C43 | −24.1 (3) |
C34B—C35B—C36—C35A | 9 (4) | C38—C37—P4—S4 | −93.0 (4) |
C32—C31—C36—C35B | 9 (3) | C42—C37—P4—S4 | 90.7 (3) |
P3—C31—C36—C35B | −169 (3) | N1—P1—S1—Pt1 | −57.10 (12) |
C32—C31—C36—C35A | −2.6 (11) | C1—P1—S1—Pt1 | 71.94 (12) |
P3—C31—C36—C35A | 179.7 (9) | C7—P1—S1—Pt1 | −173.53 (11) |
C34A—C35A—C36—C35B | −154 (6) | N2—P2—S2—Pt1 | −52.29 (15) |
C34A—C35A—C36—C31 | 6 (2) | C13—P2—S2—Pt1 | −172.08 (13) |
C42—C37—C38—C39 | −0.4 (7) | C19—P2—S2—Pt1 | 74.98 (15) |
P4—C37—C38—C39 | −176.8 (5) | N2—P3—S3—Pt1 | 51.52 (15) |
C37—C38—C39—C40 | −1.4 (10) | C25—P3—S3—Pt1 | 170.28 (14) |
C38—C39—C40—C41 | 2.6 (10) | C31—P3—S3—Pt1 | −76.69 (14) |
C39—C40—C41—C42 | −2.0 (9) | N1—P4—S4—Pt1 | −51.14 (13) |
C40—C41—C42—C37 | 0.2 (7) | C43—P4—S4—Pt1 | −171.57 (11) |
C38—C37—C42—C41 | 0.9 (6) | C37—P4—S4—Pt1 | 73.80 (13) |
P4—C37—C42—C41 | 177.3 (3) | P2—S2—Pt1—S1 | −118.08 (5) |
C48—C43—C44—C45 | −1.2 (6) | P2—S2—Pt1—S3 | 65.56 (5) |
P4—C43—C44—C45 | −178.9 (4) | P1—S1—Pt1—S2 | −161.21 (5) |
C43—C44—C45—C46 | −0.1 (7) | P1—S1—Pt1—S4 | 11.37 (5) |
C44—C45—C46—C47 | 1.2 (7) | P3—S3—Pt1—S2 | −64.69 (5) |
C45—C46—C47—C48 | −1.1 (7) | P3—S3—Pt1—S4 | 122.34 (5) |
C44—C43—C48—C47 | 1.4 (5) | P4—S4—Pt1—S1 | 32.08 (5) |
P4—C43—C48—C47 | 179.1 (3) | P4—S4—Pt1—S3 | −152.41 (5) |
C46—C47—C48—C43 | −0.2 (6) |
Experimental details
Crystal data | |
Chemical formula | [Pt(C24H20NP2S2)2] |
Mr | 1092.03 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 10.1103 (4), 10.7023 (4), 23.9258 (9) |
α, β, γ (°) | 98.137 (3), 90.496 (3), 115.563 (3) |
V (Å3) | 2304.86 (15) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 3.40 |
Crystal size (mm) | 0.56 × 0.32 × 0.08 |
Data collection | |
Diffractometer | Stoe IPDS 2 diffractometer |
Absorption correction | Integration (X-RED32; Stoe & Cie, 2002) |
Tmin, Tmax | 0.302, 0.790 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 23061, 9495, 8823 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.628 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.066, 1.03 |
No. of reflections | 9495 |
No. of parameters | 570 |
No. of restraints | 24 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.82, −0.79 |
Computer programs: X-AREA (Stoe & Cie, 2002), X-RED32 (Stoe & Cie, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
Acknowledgements
We thank Ondokuz Mayis University for their X-ray crystallography support and the Research Foundation of Ege University for funding (2009 FEN 032).
References
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In bis(diphenylphosphino)amine (dppa) ligands the phosphorous (III) atoms are succeptable to oxidation by chalcogene atoms (i.e. oxygene, sulfur and selenium). Further, double oxidation of dppa will generate bis(diphenylthiophosphoryl)-amine ligands [Ph2P(E)NHP(E)Ph2] (E= O, S, Se) and can act as a bidentate chelating anion (imidobis(diphenylthiophosphinato) with the loss of an amino proton to a metal metal ion (Schmidpeter & Groger, 1966). Similar compounds containing [R2P(E)N]2N- (R = alkyl and phenyl) have been investigated (Woollins, 1996; Haiduc, 1997; Silvestru et al., 1998). [R2P(E)N]2N- ligands can also bonded to the metal atoms as a tridentate ligand through the two chalcogene and N atoms (Sekar & Ibers, 2006). Metal complexes of imidodiphosphino dichalcogenide ligands have been widely used as precursors for the thin films, nanoparticles (Crouch et al., 2003). Iodine adducts of these ligands are used to activate the metals (Abbati et al., 2001).
In the title complex, [Pt(Ph2P(S)N(S)Ph2)] or [Pt(dppaS2)2] where dppaS2 is bis[(imidobis(diphenylthiophosphinato)]platinum(II), the Pt atom is in a distorted square planar environment with angles trans S1—Pt1—S3 [172.37 (3)°] and S2—Pt1—S4 [171.72 (3)°] and S4—Pt1—S1 and S3—Pt1—S2 bite angles of 101.45 (3)° and 90.87 (3)°, respectively (Fig. 1). These values are comparable with literature values of related compounds [Yanar et al., 2007; Bhattacharyya & Woollins, 1995]. The differences in the bite angles of S—Pt—S are likely due to the conformations of the six-membered metallo rings. In the Pt1/S1/P1/N1/P4/S4 ring, the Pt1—S1—P1—N1 and Pt1—S4—P4—N1 torsion angles are -57.12 (13)° and -51.12 (14)°, respectively, with ring puckering parameters of θ= 89.31 (11)° and Φ= 287.34 (13)°. This supports a twist-boat conformation (Cremer & Pople,1975). In the Pt1/S2/P2/N2/P3/S3 ring with Pt1—S2—P2—N2 [-52.27 (16)°] and Pt1—S3—P3—N2 [51.49 (17)°] torsion angles and ring puckering parameters of θ= 180.52 (12)° and Φ= 141.81 (12)° (Cremer & Pople, 1975) supports a half-chair conformation. The four Pt—S bond lengths are slightly different from each other [Pt1—S1: 2.3284 (9) Å, Pt1—S2: 2.3207 (8) Å, Pt1—S3: 2.3300 (9) Å, Pt1—S4: 2.3341 (8) Å]. These values are comparable with literature values [Yanar et al., 2007; İrişli & Yanar, 2006]. The observed P1—S1, P2—S2, P3—S3 and P4—S4 lengths [2.0279 (12) Å, 2.0332 (13) Å, 2.0327 (14)Å and 2.0304 (12) Å] are closer to single bond than double bond lengths (Berry et al., 1988).
Positional disorder in the aromatic rings attached to the P2 and P3 atoms occur with sof values of 0.721 (13) (C23A, C24A), 0.279 (13) (C23B, C24B), 0.71 (7) (C34A, C35A) and 0.29 (7) (C34B, C35B), respectively.