metal-organic compounds
{μ-N-[(Diphenylphosphino)methyl]pyridin-2-amine-κ2N1:P}bis{[2-(2,2′-bipyridin-6-yl)phenyl-κ3N,N′,C1]platinum(II)} bis(perchlorate)
aCollege of Animal Husbandry and Veterinary Studies, Henan Agricultural University, Zhengzhou, Henan 450002, People's Republic of China
*Correspondence e-mail: mojuan52@126.com
The title compound, [Pt2(C16H11N2)2(C18H17N2P)](ClO4)2, contains two PtII atoms, bridged by an N-[(diphenylphosphino)methyl]pyridin-2-amine (dppmp) ligand. One Pt atom is coordinated by one P atom from the dppmp ligand, and one C atom and two N atoms from a 6-phenyl-2,2′-bipyridine (pbpy) ligand in a square-planar geometry. The other Pt atom is coordinated by one N atom from the dppmp ligand, and one C atom and two N atoms from another pbpy ligand in a square-planar geometry. There are intramolecular π–π interactions between the pbpy ligands, with a centroid–centroid distance of 3.62 (1) Å between two pyridyl rings. The oxygen atoms of both perchlorate anions are disordered, each over two different positions [occupanicies 0.49 (3)/0.51 (3) and 0.48 (2)/0.52 (2)].
Related literature
For related literature, see: Braunstein et al. (1997); Catalano et al. (2001); Durran et al. (2000); Field et al. (1997); Kuang et al. (1998); Li et al. (1996); Newkome (1993).
Experimental
Crystal data
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Refinement
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Data collection: SMART (Bruker, 2007); cell SAINT (Bruker, 2007); data reduction: SAINT; 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.
Supporting information
10.1107/S1600536808024525/hy2138sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808024525/hy2138Isup2.hkl
A solution of K2(PtCl4) (0.088 g, 0.212 mmol) in water (5 ml) was treated with a solution of pbpy (0.052 g, 0.224 mmol) in MeCN (5 ml) and the mixture was heated to reflux for 20 h, allowing MeCN to evaporate slowly. The orange solid so obtained was collected by filtration, washed with water and water–EtOH (5:l, v/v) and dried in vacuo, yielding Pt(pbpy)Cl (yield 91%, 0.089 g). A 15 ml MeCN solution of Pt(pbpy)Cl (0.046 g, 0.1 mmol) was added to a 20 ml MeCN solution of dppmp (0.015 g, 0.05 mmol). The mixture was stirred for 10 h and then LiClO4 (0.021 g, 0.2 mmol) was added. Yellow crystals suitable for X-ray diffraction were formed by vapour diffusion of diethyl ether into the MeCN solution.
H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 (aromatic) and 0.97 (CH2) Å, and N—H = 0.86 Å, and with Uiso(H) = 1.2Ueq(C,N). The highest residual electron density was found 0.98 Å from atom Pt2 and the deepest hole 1.00 Å from atom Pt2. Each perchlorate anion is disordered over two different orientations. The Cl—O distances were restrained to 1.44 (3) Å.
Data collection: SMART (Bruker, 2007); cell
SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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).[Pt2(C16H11N2)2(C18H17N2P)](ClO4)2 | F(000) = 2600 |
Mr = 1343.92 | Dx = 1.928 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 7716 reflections |
a = 14.845 (3) Å | θ = 2.3–26.6° |
b = 17.927 (4) Å | µ = 6.25 mm−1 |
c = 18.481 (4) Å | T = 294 K |
β = 109.697 (3)° | Block, yellow |
V = 4630.5 (18) Å3 | 0.40 × 0.20 × 0.10 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 8097 independent reflections |
Radiation source: fine-focus sealed tube | 5253 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.090 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −17→16 |
Tmin = 0.225, Tmax = 0.534 | k = −17→21 |
22850 measured reflections | l = −20→21 |
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)] = 0.075 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.219 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0656P)2 + 39.0816P] where P = (Fo2 + 2Fc2)/3 |
8097 reflections | (Δ/σ)max = 0.001 |
696 parameters | Δρmax = 2.85 e Å−3 |
16 restraints | Δρmin = −2.38 e Å−3 |
[Pt2(C16H11N2)2(C18H17N2P)](ClO4)2 | V = 4630.5 (18) Å3 |
Mr = 1343.92 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 14.845 (3) Å | µ = 6.25 mm−1 |
b = 17.927 (4) Å | T = 294 K |
c = 18.481 (4) Å | 0.40 × 0.20 × 0.10 mm |
β = 109.697 (3)° |
Bruker SMART APEX CCD area-detector diffractometer | 8097 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 5253 reflections with I > 2σ(I) |
Tmin = 0.225, Tmax = 0.534 | Rint = 0.090 |
22850 measured reflections |
R[F2 > 2σ(F2)] = 0.075 | 16 restraints |
wR(F2) = 0.219 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0656P)2 + 39.0816P] where P = (Fo2 + 2Fc2)/3 |
8097 reflections | Δρmax = 2.85 e Å−3 |
696 parameters | Δρmin = −2.38 e Å−3 |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pt1 | 0.96899 (4) | 0.15372 (3) | 0.47609 (3) | 0.0324 (2) | |
Pt2 | 0.71657 (4) | 0.21672 (3) | 0.51620 (3) | 0.0326 (2) | |
P1 | 0.7571 (3) | 0.3339 (2) | 0.55627 (19) | 0.0325 (8) | |
N1 | 0.9510 (9) | 0.1645 (8) | 0.3600 (6) | 0.040 (3) | |
N2 | 0.8943 (8) | 0.0657 (8) | 0.4355 (6) | 0.033 (3) | |
N3 | 1.0503 (9) | 0.2462 (8) | 0.5165 (5) | 0.038 (3) | |
N4 | 0.9260 (9) | 0.3020 (8) | 0.5450 (7) | 0.040 (3) | |
H4 | 0.9029 | 0.2582 | 0.5464 | 0.048* | |
N5 | 0.7113 (10) | 0.1553 (8) | 0.6155 (8) | 0.047 (3) | |
N6 | 0.6669 (8) | 0.1175 (7) | 0.4717 (7) | 0.033 (3) | |
C1 | 0.9763 (13) | 0.2199 (10) | 0.3226 (9) | 0.047 (4) | |
H1 | 1.0069 | 0.2613 | 0.3504 | 0.056* | |
C2 | 0.9588 (14) | 0.2184 (12) | 0.2437 (10) | 0.060 (5) | |
H2 | 0.9781 | 0.2579 | 0.2198 | 0.072* | |
C3 | 0.9137 (15) | 0.1595 (13) | 0.2027 (9) | 0.065 (6) | |
H3 | 0.9037 | 0.1572 | 0.1503 | 0.078* | |
C4 | 0.8816 (12) | 0.1013 (11) | 0.2385 (9) | 0.053 (5) | |
H4A | 0.8477 | 0.0616 | 0.2095 | 0.064* | |
C5 | 0.9009 (11) | 0.1032 (9) | 0.3175 (8) | 0.040 (4) | |
C6 | 0.8704 (10) | 0.0466 (10) | 0.3612 (7) | 0.039 (4) | |
C7 | 0.8170 (11) | −0.0157 (11) | 0.3327 (9) | 0.053 (5) | |
H7 | 0.7987 | −0.0268 | 0.2806 | 0.063* | |
C8 | 0.7905 (12) | −0.0622 (11) | 0.3821 (10) | 0.056 (5) | |
H8 | 0.7547 | −0.1050 | 0.3638 | 0.068* | |
C9 | 0.8179 (10) | −0.0437 (10) | 0.4582 (9) | 0.042 (4) | |
H9 | 0.7979 | −0.0733 | 0.4912 | 0.050* | |
C10 | 0.8741 (10) | 0.0176 (9) | 0.4873 (7) | 0.034 (3) | |
C11 | 0.9076 (10) | 0.0489 (9) | 0.5636 (8) | 0.035 (3) | |
C12 | 0.8939 (11) | 0.0107 (11) | 0.6275 (8) | 0.047 (4) | |
H12 | 0.8600 | −0.0338 | 0.6203 | 0.056* | |
C13 | 0.9321 (14) | 0.0416 (13) | 0.6992 (9) | 0.063 (5) | |
H13 | 0.9226 | 0.0182 | 0.7409 | 0.076* | |
C14 | 0.9833 (13) | 0.1055 (13) | 0.7101 (9) | 0.061 (5) | |
H14 | 1.0103 | 0.1242 | 0.7597 | 0.073* | |
C15 | 0.9969 (12) | 0.1443 (10) | 0.6490 (8) | 0.045 (4) | |
H15 | 1.0298 | 0.1894 | 0.6580 | 0.054* | |
C16 | 0.9616 (9) | 0.1158 (11) | 0.5751 (7) | 0.042 (4) | |
C17 | 1.1411 (10) | 0.2502 (11) | 0.5117 (9) | 0.044 (4) | |
H17 | 1.1649 | 0.2090 | 0.4933 | 0.053* | |
C18 | 1.1961 (13) | 0.3111 (10) | 0.5326 (10) | 0.049 (4) | |
H18 | 1.2581 | 0.3103 | 0.5311 | 0.059* | |
C19 | 1.1611 (10) | 0.3767 (10) | 0.5568 (8) | 0.041 (4) | |
H19 | 1.1970 | 0.4203 | 0.5681 | 0.049* | |
C20 | 1.0709 (11) | 0.3726 (9) | 0.5628 (7) | 0.039 (4) | |
H20 | 1.0464 | 0.4131 | 0.5814 | 0.047* | |
C21 | 1.0161 (10) | 0.3071 (9) | 0.5406 (6) | 0.030 (3) | |
C22 | 0.8681 (9) | 0.3651 (9) | 0.5475 (8) | 0.034 (3) | |
H22A | 0.8554 | 0.3943 | 0.5009 | 0.041* | |
H22B | 0.9018 | 0.3965 | 0.5909 | 0.041* | |
C23 | 0.7700 (12) | 0.3500 (8) | 0.6562 (8) | 0.040 (4) | |
C24 | 0.8588 (12) | 0.3455 (11) | 0.7132 (9) | 0.054 (5) | |
H24 | 0.9141 | 0.3432 | 0.7003 | 0.065* | |
C25 | 0.8646 (16) | 0.3446 (13) | 0.7892 (10) | 0.077 (7) | |
H25 | 0.9242 | 0.3390 | 0.8271 | 0.092* | |
C26 | 0.7854 (14) | 0.3515 (12) | 0.8103 (10) | 0.059 (5) | |
H26 | 0.7902 | 0.3514 | 0.8618 | 0.070* | |
C27 | 0.6987 (15) | 0.3588 (12) | 0.7532 (9) | 0.064 (6) | |
H27 | 0.6440 | 0.3635 | 0.7666 | 0.077* | |
C28 | 0.6894 (13) | 0.3592 (12) | 0.6757 (9) | 0.055 (5) | |
H28 | 0.6298 | 0.3656 | 0.6380 | 0.067* | |
C29 | 0.6740 (10) | 0.4050 (9) | 0.5055 (7) | 0.035 (3) | |
C30 | 0.5850 (11) | 0.3829 (11) | 0.4536 (7) | 0.043 (4) | |
H30 | 0.5689 | 0.3328 | 0.4450 | 0.051* | |
C31 | 0.5226 (16) | 0.4377 (15) | 0.4159 (10) | 0.074 (7) | |
H31 | 0.4637 | 0.4239 | 0.3807 | 0.089* | |
C32 | 0.5421 (17) | 0.5077 (13) | 0.4274 (12) | 0.072 (7) | |
H32 | 0.4966 | 0.5432 | 0.4022 | 0.086* | |
C33 | 0.6317 (15) | 0.5307 (12) | 0.4777 (13) | 0.069 (6) | |
H33 | 0.6462 | 0.5813 | 0.4842 | 0.083* | |
C34 | 0.6956 (13) | 0.4806 (10) | 0.5160 (10) | 0.048 (4) | |
H34 | 0.7547 | 0.4959 | 0.5498 | 0.058* | |
C35 | 0.7382 (16) | 0.1770 (13) | 0.6886 (10) | 0.067 (6) | |
H35 | 0.7650 | 0.2241 | 0.7019 | 0.080* | |
C36 | 0.7269 (18) | 0.1308 (15) | 0.7452 (13) | 0.081 (7) | |
H36 | 0.7504 | 0.1458 | 0.7963 | 0.097* | |
C37 | 0.6828 (16) | 0.0650 (16) | 0.7270 (13) | 0.085 (8) | |
H37 | 0.6692 | 0.0361 | 0.7638 | 0.102* | |
C38 | 0.6578 (15) | 0.0413 (13) | 0.6510 (12) | 0.070 (6) | |
H38 | 0.6328 | −0.0062 | 0.6375 | 0.084* | |
C39 | 0.6702 (11) | 0.0888 (9) | 0.5949 (9) | 0.044 (4) | |
C40 | 0.6436 (12) | 0.0660 (11) | 0.5145 (11) | 0.055 (5) | |
C41 | 0.6049 (13) | −0.0013 (11) | 0.4835 (11) | 0.059 (5) | |
H41 | 0.5944 | −0.0383 | 0.5151 | 0.070* | |
C42 | 0.5824 (13) | −0.0137 (12) | 0.4087 (13) | 0.065 (6) | |
H42 | 0.5563 | −0.0591 | 0.3875 | 0.078* | |
C43 | 0.5988 (13) | 0.0432 (12) | 0.3620 (12) | 0.066 (6) | |
H43 | 0.5805 | 0.0366 | 0.3091 | 0.079* | |
C44 | 0.6428 (10) | 0.1095 (10) | 0.3956 (9) | 0.042 (4) | |
C45 | 0.6726 (11) | 0.1717 (10) | 0.3581 (8) | 0.038 (4) | |
C46 | 0.6645 (13) | 0.1717 (12) | 0.2834 (9) | 0.056 (5) | |
H46 | 0.6359 | 0.1316 | 0.2523 | 0.068* | |
C47 | 0.6988 (14) | 0.2316 (14) | 0.2526 (9) | 0.067 (6) | |
H47 | 0.6976 | 0.2300 | 0.2019 | 0.081* | |
C48 | 0.7345 (13) | 0.2930 (12) | 0.2973 (9) | 0.060 (5) | |
H48 | 0.7558 | 0.3339 | 0.2765 | 0.072* | |
C49 | 0.7389 (12) | 0.2942 (11) | 0.3716 (8) | 0.049 (4) | |
H49 | 0.7612 | 0.3374 | 0.3999 | 0.059* | |
C50 | 0.7124 (10) | 0.2355 (9) | 0.4077 (7) | 0.034 (4) | |
Cl1 | 0.9289 (4) | 0.2821 (3) | 0.0174 (3) | 0.0685 (14) | |
Cl2 | 0.4595 (5) | 0.0612 (3) | 0.8325 (2) | 0.0868 (19) | |
O1 | 0.8360 (8) | 0.3152 (11) | 0.0026 (12) | 0.045 (7) | 0.49 (3) |
O2 | 0.9880 (13) | 0.3037 (16) | 0.0961 (7) | 0.085 (11) | 0.49 (3) |
O3 | 0.9732 (14) | 0.3115 (14) | −0.0339 (11) | 0.066 (10) | 0.49 (3) |
O4 | 0.9225 (17) | 0.2030 (5) | 0.0144 (18) | 0.099 (12) | 0.49 (3) |
O1' | 0.8580 (14) | 0.3177 (12) | 0.0424 (16) | 0.084 (10) | 0.51 (3) |
O2' | 0.9950 (14) | 0.2415 (15) | 0.0795 (12) | 0.115 (12) | 0.51 (3) |
O3' | 0.9770 (13) | 0.3359 (10) | −0.0133 (11) | 0.043 (6) | 0.51 (3) |
O4' | 0.8809 (18) | 0.2289 (13) | −0.0433 (12) | 0.105 (12) | 0.51 (3) |
O5 | 0.5418 (15) | 0.0136 (14) | 0.8519 (16) | 0.126 (14) | 0.52 (2) |
O6 | 0.465 (2) | 0.1108 (12) | 0.8945 (10) | 0.089 (10) | 0.52 (2) |
O7 | 0.452 (2) | 0.1028 (12) | 0.7643 (9) | 0.070 (9) | 0.52 (2) |
O8 | 0.3747 (15) | 0.0152 (14) | 0.8177 (17) | 0.150 (17) | 0.52 (2) |
O5' | 0.4931 (16) | −0.0120 (7) | 0.8234 (11) | 0.058 (8) | 0.48 (2) |
O6' | 0.5415 (14) | 0.1089 (12) | 0.8684 (15) | 0.125 (15) | 0.48 (2) |
O7' | 0.4045 (15) | 0.0923 (11) | 0.7596 (8) | 0.052 (7) | 0.48 (2) |
O8' | 0.4025 (19) | 0.0581 (17) | 0.8818 (14) | 0.163 (18) | 0.48 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.0415 (4) | 0.0279 (4) | 0.0241 (3) | 0.0019 (2) | 0.0060 (2) | −0.0019 (2) |
Pt2 | 0.0420 (4) | 0.0225 (4) | 0.0301 (3) | −0.0007 (2) | 0.0079 (2) | −0.0017 (2) |
P1 | 0.044 (2) | 0.025 (2) | 0.0253 (17) | 0.0033 (17) | 0.0066 (14) | −0.0016 (14) |
N1 | 0.057 (8) | 0.037 (9) | 0.030 (6) | −0.001 (7) | 0.021 (6) | −0.006 (5) |
N2 | 0.035 (7) | 0.039 (8) | 0.020 (5) | −0.002 (6) | 0.003 (4) | 0.002 (5) |
N3 | 0.048 (7) | 0.049 (9) | 0.013 (5) | 0.001 (7) | 0.004 (5) | −0.001 (5) |
N4 | 0.046 (8) | 0.034 (8) | 0.044 (7) | −0.011 (6) | 0.021 (6) | −0.007 (6) |
N5 | 0.046 (8) | 0.033 (9) | 0.059 (9) | 0.000 (6) | 0.012 (6) | 0.006 (6) |
N6 | 0.030 (7) | 0.026 (7) | 0.044 (7) | 0.009 (5) | 0.014 (5) | −0.007 (5) |
C1 | 0.066 (11) | 0.035 (11) | 0.040 (8) | −0.002 (9) | 0.019 (7) | 0.003 (7) |
C2 | 0.078 (13) | 0.064 (16) | 0.047 (10) | 0.018 (11) | 0.032 (9) | 0.021 (9) |
C3 | 0.087 (14) | 0.078 (17) | 0.026 (8) | 0.003 (12) | 0.014 (8) | −0.005 (9) |
C4 | 0.066 (11) | 0.042 (12) | 0.041 (9) | 0.015 (9) | 0.003 (7) | −0.006 (8) |
C5 | 0.052 (9) | 0.029 (9) | 0.034 (7) | 0.017 (8) | 0.009 (6) | −0.002 (6) |
C6 | 0.040 (8) | 0.047 (11) | 0.027 (7) | 0.018 (8) | 0.006 (6) | −0.006 (6) |
C7 | 0.050 (10) | 0.055 (13) | 0.041 (9) | 0.004 (9) | −0.001 (7) | −0.016 (8) |
C8 | 0.060 (11) | 0.037 (11) | 0.059 (11) | −0.012 (9) | 0.004 (8) | −0.019 (8) |
C9 | 0.037 (8) | 0.033 (10) | 0.063 (10) | −0.002 (7) | 0.025 (7) | 0.005 (7) |
C10 | 0.044 (8) | 0.023 (8) | 0.034 (7) | 0.003 (7) | 0.011 (6) | 0.006 (6) |
C11 | 0.035 (8) | 0.033 (9) | 0.035 (7) | 0.005 (7) | 0.008 (6) | 0.006 (6) |
C12 | 0.043 (9) | 0.054 (12) | 0.041 (8) | 0.001 (8) | 0.010 (7) | 0.013 (8) |
C13 | 0.082 (13) | 0.074 (16) | 0.034 (9) | 0.002 (12) | 0.020 (8) | 0.015 (9) |
C14 | 0.075 (13) | 0.078 (17) | 0.028 (8) | −0.007 (12) | 0.013 (7) | −0.003 (8) |
C15 | 0.061 (10) | 0.043 (11) | 0.026 (7) | −0.002 (8) | 0.009 (7) | 0.003 (6) |
C16 | 0.017 (7) | 0.079 (14) | 0.026 (7) | 0.000 (8) | 0.002 (5) | −0.015 (7) |
C17 | 0.035 (9) | 0.052 (12) | 0.059 (9) | 0.011 (8) | 0.033 (7) | 0.011 (8) |
C18 | 0.055 (10) | 0.027 (10) | 0.063 (10) | −0.002 (8) | 0.015 (8) | 0.004 (7) |
C19 | 0.031 (8) | 0.043 (11) | 0.043 (8) | −0.020 (7) | 0.006 (6) | −0.001 (7) |
C20 | 0.059 (10) | 0.023 (9) | 0.027 (7) | −0.013 (7) | 0.002 (6) | −0.004 (6) |
C21 | 0.039 (8) | 0.034 (9) | 0.015 (6) | 0.001 (7) | 0.005 (5) | −0.010 (5) |
C22 | 0.031 (8) | 0.046 (10) | 0.028 (7) | 0.004 (7) | 0.013 (6) | −0.002 (6) |
C23 | 0.069 (11) | 0.012 (8) | 0.033 (7) | 0.003 (7) | 0.008 (7) | −0.010 (5) |
C24 | 0.050 (10) | 0.068 (15) | 0.039 (9) | −0.005 (9) | 0.009 (7) | 0.000 (8) |
C25 | 0.095 (16) | 0.085 (19) | 0.029 (9) | −0.025 (13) | −0.007 (9) | −0.012 (9) |
C26 | 0.079 (14) | 0.062 (15) | 0.037 (9) | −0.010 (11) | 0.022 (9) | −0.016 (8) |
C27 | 0.094 (15) | 0.067 (16) | 0.037 (9) | 0.004 (11) | 0.031 (9) | −0.007 (8) |
C28 | 0.062 (11) | 0.064 (14) | 0.040 (9) | 0.031 (10) | 0.017 (8) | 0.011 (8) |
C29 | 0.041 (8) | 0.033 (10) | 0.028 (7) | 0.016 (7) | 0.009 (6) | 0.003 (6) |
C30 | 0.053 (10) | 0.051 (12) | 0.021 (7) | 0.013 (8) | 0.008 (6) | −0.004 (6) |
C31 | 0.092 (15) | 0.09 (2) | 0.035 (9) | 0.043 (14) | 0.015 (9) | 0.016 (10) |
C32 | 0.098 (17) | 0.050 (15) | 0.083 (14) | 0.053 (13) | 0.050 (13) | 0.046 (11) |
C33 | 0.084 (15) | 0.048 (15) | 0.096 (15) | 0.008 (12) | 0.058 (13) | 0.039 (12) |
C34 | 0.066 (11) | 0.031 (11) | 0.063 (10) | 0.018 (8) | 0.042 (9) | 0.016 (8) |
C35 | 0.111 (16) | 0.051 (13) | 0.036 (9) | 0.010 (12) | 0.021 (9) | 0.015 (8) |
C36 | 0.123 (19) | 0.067 (17) | 0.065 (13) | −0.010 (15) | 0.048 (13) | 0.026 (11) |
C37 | 0.094 (16) | 0.09 (2) | 0.083 (16) | 0.003 (14) | 0.044 (13) | 0.055 (14) |
C38 | 0.092 (15) | 0.041 (13) | 0.081 (14) | −0.008 (11) | 0.034 (11) | 0.006 (10) |
C39 | 0.046 (9) | 0.024 (9) | 0.063 (10) | 0.002 (7) | 0.020 (7) | 0.000 (7) |
C40 | 0.047 (10) | 0.033 (11) | 0.070 (11) | −0.004 (8) | 0.001 (8) | −0.015 (9) |
C41 | 0.068 (12) | 0.028 (11) | 0.075 (12) | 0.014 (9) | 0.018 (9) | −0.003 (9) |
C42 | 0.049 (11) | 0.039 (13) | 0.106 (16) | −0.006 (9) | 0.022 (10) | −0.020 (11) |
C43 | 0.058 (11) | 0.044 (13) | 0.074 (12) | −0.003 (10) | −0.007 (9) | −0.037 (10) |
C44 | 0.027 (8) | 0.044 (11) | 0.048 (9) | 0.007 (7) | 0.005 (6) | −0.009 (7) |
C45 | 0.041 (9) | 0.036 (10) | 0.026 (7) | 0.007 (7) | −0.002 (6) | −0.003 (6) |
C46 | 0.069 (12) | 0.051 (13) | 0.029 (8) | 0.026 (10) | −0.010 (7) | −0.013 (8) |
C47 | 0.084 (14) | 0.083 (18) | 0.026 (8) | 0.039 (13) | 0.007 (8) | 0.007 (9) |
C48 | 0.071 (12) | 0.053 (13) | 0.043 (9) | 0.020 (10) | 0.004 (8) | 0.006 (8) |
C49 | 0.065 (11) | 0.050 (12) | 0.026 (7) | −0.016 (9) | 0.006 (7) | 0.001 (7) |
C50 | 0.034 (8) | 0.040 (10) | 0.030 (7) | 0.008 (7) | 0.012 (6) | −0.020 (6) |
Cl1 | 0.070 (3) | 0.057 (4) | 0.091 (4) | 0.007 (3) | 0.044 (3) | 0.023 (3) |
Cl2 | 0.158 (6) | 0.043 (3) | 0.038 (2) | 0.008 (3) | 0.005 (3) | 0.000 (2) |
O1 | 0.043 (10) | 0.049 (11) | 0.046 (10) | −0.003 (8) | 0.021 (7) | −0.006 (7) |
O2 | 0.092 (13) | 0.083 (14) | 0.076 (13) | 0.002 (9) | 0.022 (9) | 0.009 (9) |
O3 | 0.071 (12) | 0.066 (13) | 0.059 (12) | −0.008 (9) | 0.021 (8) | −0.007 (9) |
O4 | 0.099 (14) | 0.097 (15) | 0.110 (15) | 0.004 (9) | 0.046 (10) | 0.002 (9) |
O1' | 0.080 (13) | 0.087 (14) | 0.088 (13) | −0.008 (9) | 0.033 (9) | −0.001 (9) |
O2' | 0.119 (14) | 0.116 (15) | 0.112 (14) | 0.010 (9) | 0.041 (10) | 0.016 (9) |
O3' | 0.043 (9) | 0.042 (10) | 0.043 (9) | −0.010 (7) | 0.014 (7) | −0.008 (8) |
O4' | 0.104 (14) | 0.105 (16) | 0.107 (15) | −0.004 (9) | 0.034 (10) | −0.001 (9) |
O5 | 0.123 (16) | 0.120 (17) | 0.129 (16) | 0.006 (10) | 0.034 (10) | 0.009 (10) |
O6 | 0.100 (13) | 0.085 (13) | 0.073 (12) | −0.003 (9) | 0.018 (8) | −0.013 (9) |
O7 | 0.081 (12) | 0.055 (12) | 0.067 (11) | −0.005 (9) | 0.018 (8) | 0.012 (8) |
O8 | 0.153 (18) | 0.143 (19) | 0.144 (19) | −0.007 (10) | 0.038 (10) | 0.002 (10) |
O5' | 0.069 (11) | 0.046 (11) | 0.047 (10) | 0.006 (8) | 0.003 (7) | −0.001 (8) |
O6' | 0.129 (17) | 0.118 (17) | 0.120 (17) | −0.004 (10) | 0.030 (10) | −0.006 (10) |
O7' | 0.043 (10) | 0.047 (11) | 0.057 (10) | −0.002 (8) | 0.007 (7) | 0.006 (8) |
O8' | 0.167 (19) | 0.17 (2) | 0.161 (19) | 0.005 (10) | 0.062 (11) | 0.007 (10) |
Pt1—N2 | 1.928 (13) | C24—C25 | 1.38 (2) |
Pt1—C16 | 1.990 (15) | C24—H24 | 0.9300 |
Pt1—N3 | 2.038 (14) | C25—C26 | 1.36 (3) |
Pt1—N1 | 2.079 (11) | C25—H25 | 0.9300 |
Pt2—N6 | 1.993 (13) | C26—C27 | 1.37 (3) |
Pt2—C50 | 2.014 (14) | C26—H26 | 0.9300 |
Pt2—N5 | 2.164 (14) | C27—C28 | 1.39 (2) |
Pt2—P1 | 2.241 (4) | C27—H27 | 0.9300 |
P1—C22 | 1.799 (14) | C28—H28 | 0.9300 |
P1—C29 | 1.802 (14) | C29—C34 | 1.39 (2) |
P1—C23 | 1.814 (14) | C29—C30 | 1.40 (2) |
N1—C1 | 1.34 (2) | C30—C31 | 1.37 (3) |
N1—C5 | 1.41 (2) | C30—H30 | 0.9300 |
N2—C6 | 1.342 (17) | C31—C32 | 1.29 (3) |
N2—C10 | 1.394 (18) | C31—H31 | 0.9300 |
N3—C21 | 1.342 (19) | C32—C33 | 1.40 (3) |
N3—C17 | 1.381 (19) | C32—H32 | 0.9300 |
N4—C21 | 1.370 (18) | C33—C34 | 1.33 (2) |
N4—C22 | 1.43 (2) | C33—H33 | 0.9300 |
N4—H4 | 0.8600 | C34—H34 | 0.9300 |
N5—C35 | 1.33 (2) | C35—C36 | 1.39 (3) |
N5—C39 | 1.34 (2) | C35—H35 | 0.9300 |
N6—C40 | 1.33 (2) | C36—C37 | 1.34 (4) |
N6—C44 | 1.338 (19) | C36—H36 | 0.9300 |
C1—C2 | 1.39 (2) | C37—C38 | 1.39 (3) |
C1—H1 | 0.9300 | C37—H37 | 0.9300 |
C2—C3 | 1.34 (3) | C38—C39 | 1.40 (3) |
C2—H2 | 0.9300 | C38—H38 | 0.9300 |
C3—C4 | 1.40 (3) | C39—C40 | 1.46 (2) |
C3—H3 | 0.9300 | C40—C41 | 1.38 (3) |
C4—C5 | 1.39 (2) | C41—C42 | 1.33 (3) |
C4—H4A | 0.9300 | C41—H41 | 0.9300 |
C5—C6 | 1.46 (2) | C42—C43 | 1.41 (3) |
C6—C7 | 1.37 (2) | C42—H42 | 0.9300 |
C7—C8 | 1.39 (3) | C43—C44 | 1.40 (2) |
C7—H7 | 0.9300 | C43—H43 | 0.9300 |
C8—C9 | 1.37 (2) | C44—C45 | 1.46 (2) |
C8—H8 | 0.9300 | C45—C46 | 1.35 (2) |
C9—C10 | 1.37 (2) | C45—C50 | 1.46 (2) |
C9—H9 | 0.9300 | C46—C47 | 1.39 (3) |
C10—C11 | 1.44 (2) | C46—H46 | 0.9300 |
C11—C16 | 1.42 (2) | C47—C48 | 1.37 (3) |
C11—C12 | 1.44 (2) | C47—H47 | 0.9300 |
C12—C13 | 1.37 (2) | C48—C49 | 1.35 (2) |
C12—H12 | 0.9300 | C48—H48 | 0.9300 |
C13—C14 | 1.35 (3) | C49—C50 | 1.37 (2) |
C13—H13 | 0.9300 | C49—H49 | 0.9300 |
C14—C15 | 1.40 (2) | Cl1—O4 | 1.421 (8) |
C14—H14 | 0.9300 | Cl1—O3 | 1.424 (8) |
C15—C16 | 1.39 (2) | Cl1—O3' | 1.427 (8) |
C15—H15 | 0.9300 | Cl1—O2' | 1.432 (8) |
C17—C18 | 1.34 (2) | Cl1—O1' | 1.434 (8) |
C17—H17 | 0.9300 | Cl1—O1 | 1.440 (8) |
C18—C19 | 1.42 (3) | Cl1—O4' | 1.461 (9) |
C18—H18 | 0.9300 | Cl1—O2 | 1.474 (8) |
C19—C20 | 1.38 (2) | Cl2—O6 | 1.430 (9) |
C19—H19 | 0.9300 | Cl2—O7' | 1.431 (8) |
C20—C21 | 1.41 (2) | Cl2—O5' | 1.434 (8) |
C20—H20 | 0.9300 | Cl2—O5 | 1.435 (9) |
C22—H22A | 0.9700 | Cl2—O7 | 1.437 (8) |
C22—H22B | 0.9700 | Cl2—O8' | 1.439 (9) |
C23—C28 | 1.37 (2) | Cl2—O6' | 1.452 (9) |
C23—C24 | 1.39 (2) | Cl2—O8 | 1.453 (9) |
N2—Pt1—C16 | 82.8 (6) | C23—C28—H28 | 120.8 |
N2—Pt1—N3 | 178.1 (4) | C27—C28—H28 | 120.8 |
C16—Pt1—N3 | 98.7 (6) | C34—C29—C30 | 119.3 (14) |
N2—Pt1—N1 | 79.5 (5) | C34—C29—P1 | 122.1 (12) |
C16—Pt1—N1 | 162.3 (6) | C30—C29—P1 | 118.6 (13) |
N3—Pt1—N1 | 99.0 (5) | C31—C30—C29 | 118 (2) |
N6—Pt2—C50 | 81.7 (6) | C31—C30—H30 | 121.1 |
N6—Pt2—N5 | 77.4 (5) | C29—C30—H30 | 121.1 |
C50—Pt2—N5 | 158.8 (6) | C32—C31—C30 | 123 (2) |
N6—Pt2—P1 | 173.4 (4) | C32—C31—H31 | 118.7 |
C50—Pt2—P1 | 95.0 (5) | C30—C31—H31 | 118.7 |
N5—Pt2—P1 | 106.2 (4) | C31—C32—C33 | 120.4 (18) |
C22—P1—C29 | 102.7 (7) | C31—C32—H32 | 119.8 |
C22—P1—C23 | 104.9 (7) | C33—C32—H32 | 119.8 |
C29—P1—C23 | 103.7 (7) | C34—C33—C32 | 120 (2) |
C22—P1—Pt2 | 114.5 (5) | C34—C33—H33 | 119.9 |
C29—P1—Pt2 | 115.5 (5) | C32—C33—H33 | 119.9 |
C23—P1—Pt2 | 114.2 (5) | C33—C34—C29 | 119.7 (19) |
C1—N1—C5 | 118.6 (13) | C33—C34—H34 | 120.1 |
C1—N1—Pt1 | 130.0 (12) | C29—C34—H34 | 120.1 |
C5—N1—Pt1 | 111.3 (10) | N5—C35—C36 | 121 (2) |
C6—N2—C10 | 120.0 (14) | N5—C35—H35 | 119.4 |
C6—N2—Pt1 | 121.8 (11) | C36—C35—H35 | 119.4 |
C10—N2—Pt1 | 117.9 (9) | C37—C36—C35 | 121 (2) |
C21—N3—C17 | 117.7 (15) | C37—C36—H36 | 119.6 |
C21—N3—Pt1 | 122.7 (10) | C35—C36—H36 | 119.6 |
C17—N3—Pt1 | 119.3 (12) | C36—C37—C38 | 117.7 (17) |
C21—N4—C22 | 123.9 (14) | C36—C37—H37 | 121.2 |
C21—N4—H4 | 118.1 | C38—C37—H37 | 121.2 |
C22—N4—H4 | 118.1 | C37—C38—C39 | 120 (2) |
C35—N5—C39 | 120.2 (15) | C37—C38—H38 | 119.9 |
C35—N5—Pt2 | 128.9 (13) | C39—C38—H38 | 119.9 |
C39—N5—Pt2 | 110.8 (11) | N5—C39—C38 | 119.5 (16) |
C40—N6—C44 | 121.2 (15) | N5—C39—C40 | 118.8 (15) |
C40—N6—Pt2 | 120.5 (11) | C38—C39—C40 | 121.7 (17) |
C44—N6—Pt2 | 117.4 (11) | N6—C40—C41 | 121.1 (18) |
N1—C1—C2 | 122.9 (18) | N6—C40—C39 | 111.9 (15) |
N1—C1—H1 | 118.6 | C41—C40—C39 | 126.9 (19) |
C2—C1—H1 | 118.6 | C42—C41—C40 | 120 (2) |
C3—C2—C1 | 119.2 (18) | C42—C41—H41 | 119.9 |
C3—C2—H2 | 120.4 | C40—C41—H41 | 119.9 |
C1—C2—H2 | 120.4 | C41—C42—C43 | 118.9 (19) |
C2—C3—C4 | 120.3 (16) | C41—C42—H42 | 120.6 |
C2—C3—H3 | 119.9 | C43—C42—H42 | 120.6 |
C4—C3—H3 | 119.9 | C44—C43—C42 | 119.6 (18) |
C5—C4—C3 | 119.6 (18) | C44—C43—H43 | 120.2 |
C5—C4—H4A | 120.2 | C42—C43—H43 | 120.2 |
C3—C4—H4A | 120.2 | N6—C44—C43 | 118.6 (17) |
C4—C5—N1 | 119.2 (16) | N6—C44—C45 | 113.6 (15) |
C4—C5—C6 | 124.8 (16) | C43—C44—C45 | 127.7 (16) |
N1—C5—C6 | 115.9 (12) | C46—C45—C44 | 123.5 (17) |
N2—C6—C7 | 121.5 (15) | C46—C45—C50 | 121.4 (17) |
N2—C6—C5 | 111.3 (15) | C44—C45—C50 | 115.2 (13) |
C7—C6—C5 | 127.0 (13) | C45—C46—C47 | 120.2 (18) |
C6—C7—C8 | 119.5 (15) | C45—C46—H46 | 119.9 |
C6—C7—H7 | 120.2 | C47—C46—H46 | 119.9 |
C8—C7—H7 | 120.2 | C48—C47—C46 | 119.6 (17) |
C9—C8—C7 | 118.6 (16) | C48—C47—H47 | 120.2 |
C9—C8—H8 | 120.7 | C46—C47—H47 | 120.2 |
C7—C8—H8 | 120.7 | C49—C48—C47 | 120 (2) |
C8—C9—C10 | 121.8 (15) | C49—C48—H48 | 119.9 |
C8—C9—H9 | 119.1 | C47—C48—H48 | 119.9 |
C10—C9—H9 | 119.1 | C48—C49—C50 | 123.8 (18) |
C9—C10—N2 | 117.9 (12) | C48—C49—H49 | 118.1 |
C9—C10—C11 | 131.1 (13) | C50—C49—H49 | 118.1 |
N2—C10—C11 | 110.3 (13) | C49—C50—C45 | 114.7 (13) |
C16—C11—C12 | 120.6 (13) | C49—C50—Pt2 | 134.0 (12) |
C16—C11—C10 | 117.9 (12) | C45—C50—Pt2 | 111.3 (12) |
C12—C11—C10 | 121.3 (15) | O4—Cl1—O3 | 112.5 (8) |
C13—C12—C11 | 118.4 (17) | O4—Cl1—O3' | 134.0 (12) |
C13—C12—H12 | 120.8 | O4—Cl1—O2' | 62.8 (14) |
C11—C12—H12 | 120.8 | O3—Cl1—O2' | 112.1 (14) |
C14—C13—C12 | 121.0 (16) | O3'—Cl1—O2' | 111.2 (8) |
C14—C13—H13 | 119.5 | O4—Cl1—O1' | 114.2 (13) |
C12—C13—H13 | 119.5 | O3—Cl1—O1' | 127.1 (13) |
C13—C14—C15 | 121.8 (15) | O3'—Cl1—O1' | 110.3 (8) |
C13—C14—H14 | 119.1 | O2'—Cl1—O1' | 110.3 (8) |
C15—C14—H14 | 119.1 | O4—Cl1—O1 | 110.9 (8) |
C16—C15—C14 | 120.3 (17) | O3—Cl1—O1 | 110.4 (8) |
C16—C15—H15 | 119.9 | O3'—Cl1—O1 | 102.8 (13) |
C14—C15—H15 | 119.9 | O2'—Cl1—O1 | 135.7 (12) |
C15—C16—C11 | 117.8 (14) | O4—Cl1—O4' | 46.4 (13) |
C15—C16—Pt1 | 131.4 (14) | O3—Cl1—O4' | 86.9 (13) |
C11—C16—Pt1 | 110.7 (9) | O3'—Cl1—O4' | 108.4 (8) |
C18—C17—N3 | 122.5 (17) | O2'—Cl1—O4' | 108.0 (8) |
C18—C17—H17 | 118.8 | O1'—Cl1—O4' | 108.5 (8) |
N3—C17—H17 | 118.8 | O1—Cl1—O4' | 86.3 (12) |
C17—C18—C19 | 120.9 (17) | O4—Cl1—O2 | 108.1 (8) |
C17—C18—H18 | 119.5 | O3—Cl1—O2 | 107.8 (8) |
C19—C18—H18 | 119.5 | O3'—Cl1—O2 | 90.2 (12) |
C20—C19—C18 | 116.7 (16) | O2'—Cl1—O2 | 47.4 (13) |
C20—C19—H19 | 121.6 | O1'—Cl1—O2 | 79.8 (12) |
C18—C19—H19 | 121.6 | O1—Cl1—O2 | 107.0 (7) |
C19—C20—C21 | 120.1 (15) | O4'—Cl1—O2 | 154.4 (13) |
C19—C20—H20 | 120.0 | O6—Cl2—O7' | 111.9 (14) |
C21—C20—H20 | 120.0 | O6—Cl2—O5' | 137.2 (13) |
N3—C21—N4 | 116.8 (14) | O7'—Cl2—O5' | 110.9 (8) |
N3—C21—C20 | 122.0 (14) | O6—Cl2—O5 | 110.9 (8) |
N4—C21—C20 | 121.2 (14) | O7'—Cl2—O5 | 129.3 (14) |
N4—C22—P1 | 109.6 (11) | O6—Cl2—O7 | 110.4 (8) |
N4—C22—H22A | 109.8 | O5'—Cl2—O7 | 107.4 (14) |
P1—C22—H22A | 109.8 | O5—Cl2—O7 | 109.5 (8) |
N4—C22—H22B | 109.8 | O6—Cl2—O8' | 53.3 (14) |
P1—C22—H22B | 109.8 | O7'—Cl2—O8' | 110.0 (8) |
H22A—C22—H22B | 108.2 | O5'—Cl2—O8' | 109.9 (8) |
C28—C23—C24 | 119.8 (14) | O5—Cl2—O8' | 116.9 (15) |
C28—C23—P1 | 119.0 (12) | O7—Cl2—O8' | 133.6 (14) |
C24—C23—P1 | 120.8 (13) | O6—Cl2—O6' | 57.0 (13) |
C25—C24—C23 | 119.6 (17) | O7'—Cl2—O6' | 109.1 (8) |
C25—C24—H24 | 120.2 | O5'—Cl2—O6' | 108.7 (8) |
C23—C24—H24 | 120.2 | O5—Cl2—O6' | 73.9 (14) |
C26—C25—C24 | 121.8 (18) | O7—Cl2—O6' | 84.2 (13) |
C26—C25—H25 | 119.1 | O8'—Cl2—O6' | 108.3 (8) |
C24—C25—H25 | 119.1 | O6—Cl2—O8 | 108.4 (8) |
C25—C26—C27 | 117.7 (16) | O7'—Cl2—O8 | 82.0 (12) |
C25—C26—H26 | 121.2 | O5'—Cl2—O8 | 76.8 (14) |
C27—C26—H26 | 121.2 | O5—Cl2—O8 | 108.6 (8) |
C26—C27—C28 | 122.5 (18) | O7—Cl2—O8 | 109.0 (8) |
C26—C27—H27 | 118.8 | O8'—Cl2—O8 | 55.9 (14) |
C28—C27—H27 | 118.8 | O6'—Cl2—O8 | 163.8 (14) |
C23—C28—C27 | 118.5 (16) | ||
C50—Pt2—P1—C22 | −59.8 (6) | Pt1—N3—C21—C20 | −175.0 (9) |
N5—Pt2—P1—C22 | 118.4 (6) | C22—N4—C21—N3 | −161.1 (12) |
C50—Pt2—P1—C29 | 59.2 (6) | C22—N4—C21—C20 | 20.9 (19) |
N5—Pt2—P1—C29 | −122.6 (6) | C19—C20—C21—N3 | 3 (2) |
C50—Pt2—P1—C23 | 179.3 (7) | C19—C20—C21—N4 | −179.1 (13) |
N5—Pt2—P1—C23 | −2.5 (7) | C21—N4—C22—P1 | −178.1 (10) |
N2—Pt1—N1—C1 | 174.6 (16) | C29—P1—C22—N4 | −148.3 (9) |
C16—Pt1—N1—C1 | 173.0 (18) | C23—P1—C22—N4 | 103.6 (10) |
N3—Pt1—N1—C1 | −6.6 (16) | Pt2—P1—C22—N4 | −22.4 (10) |
N2—Pt1—N1—C5 | −2.8 (10) | C22—P1—C23—C28 | 155.5 (14) |
C16—Pt1—N1—C5 | −4 (2) | C29—P1—C23—C28 | 48.1 (16) |
N3—Pt1—N1—C5 | 176.0 (10) | Pt2—P1—C23—C28 | −78.4 (15) |
C16—Pt1—N2—C6 | −176.1 (12) | C22—P1—C23—C24 | −31.1 (16) |
N1—Pt1—N2—C6 | 4.4 (11) | C29—P1—C23—C24 | −138.5 (14) |
C16—Pt1—N2—C10 | −2.9 (11) | Pt2—P1—C23—C24 | 95.0 (14) |
N1—Pt1—N2—C10 | 177.6 (11) | C28—C23—C24—C25 | 5 (3) |
C16—Pt1—N3—C21 | −72.3 (11) | P1—C23—C24—C25 | −168.3 (16) |
N1—Pt1—N3—C21 | 107.6 (11) | C23—C24—C25—C26 | −3 (3) |
C16—Pt1—N3—C17 | 114.7 (11) | C24—C25—C26—C27 | 1 (3) |
N1—Pt1—N3—C17 | −65.4 (11) | C25—C26—C27—C28 | 0 (3) |
N6—Pt2—N5—C35 | 177.4 (17) | C24—C23—C28—C27 | −4 (3) |
C50—Pt2—N5—C35 | 166.7 (16) | P1—C23—C28—C27 | 169.1 (16) |
P1—Pt2—N5—C35 | −8.3 (17) | C26—C27—C28—C23 | 2 (3) |
N6—Pt2—N5—C39 | −6.1 (11) | C22—P1—C29—C34 | −45.2 (13) |
C50—Pt2—N5—C39 | −17 (2) | C23—P1—C29—C34 | 63.8 (13) |
P1—Pt2—N5—C39 | 168.1 (10) | Pt2—P1—C29—C34 | −170.5 (10) |
C50—Pt2—N6—C40 | −176.6 (13) | C22—P1—C29—C30 | 134.6 (11) |
N5—Pt2—N6—C40 | 7.4 (12) | C23—P1—C29—C30 | −116.4 (12) |
C50—Pt2—N6—C44 | −7.6 (10) | Pt2—P1—C29—C30 | 9.3 (12) |
N5—Pt2—N6—C44 | 176.3 (11) | C34—C29—C30—C31 | −1 (2) |
C5—N1—C1—C2 | −3 (3) | P1—C29—C30—C31 | 179.5 (12) |
Pt1—N1—C1—C2 | −180.0 (13) | C29—C30—C31—C32 | −1 (3) |
N1—C1—C2—C3 | 1 (3) | C30—C31—C32—C33 | 3 (3) |
C1—C2—C3—C4 | 2 (3) | C31—C32—C33—C34 | −3 (3) |
C2—C3—C4—C5 | −3 (3) | C32—C33—C34—C29 | 1 (2) |
C3—C4—C5—N1 | 1 (2) | C30—C29—C34—C33 | 1 (2) |
C3—C4—C5—C6 | 179.2 (16) | P1—C29—C34—C33 | −179.5 (12) |
C1—N1—C5—C4 | 2 (2) | C39—N5—C35—C36 | 2 (3) |
Pt1—N1—C5—C4 | 179.5 (12) | Pt2—N5—C35—C36 | 178.0 (16) |
C1—N1—C5—C6 | −176.5 (14) | N5—C35—C36—C37 | −5 (4) |
Pt1—N1—C5—C6 | 1.3 (16) | C35—C36—C37—C38 | 7 (4) |
C10—N2—C6—C7 | 7 (2) | C36—C37—C38—C39 | −6 (3) |
Pt1—N2—C6—C7 | −179.7 (12) | C35—N5—C39—C38 | −2 (3) |
C10—N2—C6—C5 | −177.9 (12) | Pt2—N5—C39—C38 | −178.4 (14) |
Pt1—N2—C6—C5 | −4.7 (17) | C35—N5—C39—C40 | −178.5 (17) |
C4—C5—C6—N2 | −176.2 (14) | Pt2—N5—C39—C40 | 4.7 (19) |
N1—C5—C6—N2 | 1.9 (19) | C37—C38—C39—N5 | 4 (3) |
C4—C5—C6—C7 | −2 (3) | C37—C38—C39—C40 | −179.3 (18) |
N1—C5—C6—C7 | 176.5 (15) | C44—N6—C40—C41 | 8 (3) |
N2—C6—C7—C8 | −3 (2) | Pt2—N6—C40—C41 | 176.8 (13) |
C5—C6—C7—C8 | −177.0 (16) | C44—N6—C40—C39 | −175.5 (13) |
C6—C7—C8—C9 | 1 (3) | Pt2—N6—C40—C39 | −6.9 (19) |
C7—C8—C9—C10 | −3 (3) | N5—C39—C40—N6 | 1 (2) |
C8—C9—C10—N2 | 7 (2) | C38—C39—C40—N6 | −176.0 (16) |
C8—C9—C10—C11 | 177.0 (17) | N5—C39—C40—C41 | 176.8 (17) |
C6—N2—C10—C9 | −9 (2) | C38—C39—C40—C41 | 0 (3) |
Pt1—N2—C10—C9 | 177.6 (11) | N6—C40—C41—C42 | −6 (3) |
C6—N2—C10—C11 | 179.0 (12) | C39—C40—C41—C42 | 178.6 (18) |
Pt1—N2—C10—C11 | 5.6 (16) | C40—C41—C42—C43 | 0 (3) |
C9—C10—C11—C16 | −176.9 (16) | C41—C42—C43—C44 | 3 (3) |
N2—C10—C11—C16 | −6.3 (19) | C40—N6—C44—C43 | −5 (2) |
C9—C10—C11—C12 | 8 (3) | Pt2—N6—C44—C43 | −173.6 (12) |
N2—C10—C11—C12 | 178.9 (13) | C40—N6—C44—C45 | 179.0 (14) |
C16—C11—C12—C13 | 2 (2) | Pt2—N6—C44—C45 | 10.1 (17) |
C10—C11—C12—C13 | 176.4 (16) | C42—C43—C44—N6 | −1 (3) |
C11—C12—C13—C14 | −2 (3) | C42—C43—C44—C45 | 174.6 (17) |
C12—C13—C14—C15 | 2 (3) | N6—C44—C45—C46 | 172.9 (14) |
C13—C14—C15—C16 | −3 (3) | C43—C44—C45—C46 | −3 (3) |
C14—C15—C16—C11 | 3 (2) | N6—C44—C45—C50 | −7 (2) |
C14—C15—C16—Pt1 | −178.8 (13) | C43—C44—C45—C50 | 176.9 (15) |
C12—C11—C16—C15 | −3 (2) | C44—C45—C46—C47 | −176.8 (16) |
C10—C11—C16—C15 | −177.5 (14) | C50—C45—C46—C47 | 3 (3) |
C12—C11—C16—Pt1 | 179.0 (11) | C45—C46—C47—C48 | −5 (3) |
C10—C11—C16—Pt1 | 4.1 (17) | C46—C47—C48—C49 | 2 (3) |
N2—Pt1—C16—C15 | −178.8 (16) | C47—C48—C49—C50 | 2 (3) |
N3—Pt1—C16—C15 | 2.4 (17) | C48—C49—C50—C45 | −4 (2) |
N1—Pt1—C16—C15 | −177.2 (15) | C48—C49—C50—Pt2 | 176.0 (13) |
N2—Pt1—C16—C11 | −0.7 (11) | C46—C45—C50—C49 | 1 (2) |
N3—Pt1—C16—C11 | −179.5 (10) | C44—C45—C50—C49 | −179.1 (14) |
N1—Pt1—C16—C11 | 1 (3) | C46—C45—C50—Pt2 | −179.0 (12) |
C21—N3—C17—C18 | 2 (2) | C44—C45—C50—Pt2 | 1.2 (16) |
Pt1—N3—C17—C18 | 175.7 (12) | N6—Pt2—C50—C49 | −176.6 (17) |
N3—C17—C18—C19 | −4 (2) | N5—Pt2—C50—C49 | −165.9 (15) |
C17—C18—C19—C20 | 4 (2) | P1—Pt2—C50—C49 | 9.2 (16) |
C18—C19—C20—C21 | −4 (2) | N6—Pt2—C50—C45 | 3.1 (10) |
C17—N3—C21—N4 | −179.9 (12) | N5—Pt2—C50—C45 | 14 (2) |
Pt1—N3—C21—N4 | 6.9 (16) | P1—Pt2—C50—C45 | −171.1 (9) |
C17—N3—C21—C20 | −1.9 (19) |
Experimental details
Crystal data | |
Chemical formula | [Pt2(C16H11N2)2(C18H17N2P)](ClO4)2 |
Mr | 1343.92 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 294 |
a, b, c (Å) | 14.845 (3), 17.927 (4), 18.481 (4) |
β (°) | 109.697 (3) |
V (Å3) | 4630.5 (18) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 6.25 |
Crystal size (mm) | 0.40 × 0.20 × 0.10 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.225, 0.534 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22850, 8097, 5253 |
Rint | 0.090 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.075, 0.219, 1.03 |
No. of reflections | 8097 |
No. of parameters | 696 |
No. of restraints | 16 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0656P)2 + 39.0816P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 2.85, −2.38 |
Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Pt1—N2 | 1.928 (13) | Pt2—N6 | 1.993 (13) |
Pt1—C16 | 1.990 (15) | Pt2—C50 | 2.014 (14) |
Pt1—N3 | 2.038 (14) | Pt2—N5 | 2.164 (14) |
Pt1—N1 | 2.079 (11) | Pt2—P1 | 2.241 (4) |
N2—Pt1—C16 | 82.8 (6) | N6—Pt2—C50 | 81.7 (6) |
N2—Pt1—N3 | 178.1 (4) | N6—Pt2—N5 | 77.4 (5) |
C16—Pt1—N3 | 98.7 (6) | C50—Pt2—N5 | 158.8 (6) |
N2—Pt1—N1 | 79.5 (5) | N6—Pt2—P1 | 173.4 (4) |
C16—Pt1—N1 | 162.3 (6) | C50—Pt2—P1 | 95.0 (5) |
N3—Pt1—N1 | 99.0 (5) | N5—Pt2—P1 | 106.2 (4) |
Acknowledgements
We thank Henan Agricultural University for the generous support of this study.
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
Pyridylphosphines have induced much interest as excellent ligands with both P– and N-donor centres (Kuang et al., 1998; Newkome, 1993). These pyridylphosphines display various coordination modes: P-coordination, N-coordination, P,N-chelating and P,N-bridging (Braunstein et al., 1997; Catalano et al., 2001; Durran et al., 2000; Field et al., 1997; Li et al., 1996). Here, we report the crystal structure of the title compound, in which two PtII atoms are bridged by an N-[(diphenylphosphino)methyl]pyridin-2-amine (dppmp) ligand.
In the title compound (Fig. 1), the Pt1 atom is coordinated by one pyridyl N atom from the dppmp ligand, and one C atom and two N atoms from a 6-phenyl-2,2'-bipyridine (pbpy) ligand in a square-planar geometry (Table 1). The Pt2 atom is coordinated by one P atom from the dppmp ligand, and one C atom and two N atoms from another pbpy ligand in a square-planar geometry. The atoms Pt1, N1, N2, N3 and C16 show a mean deviation of 0.01 (1)Å from the least-squares plane through them. The planarity of the coordination geometry around the Pt2 atom was accessed by fitting a least-squares plane to the atoms Pt2, P1, N5, N6 and C50, which show a mean deviation of 0.08 (1) Å. Dihedral angle between the planes defined by two Pt atoms and the corresponding coordinated atoms is 16.6 (2)°.