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Acta Crystallogr Sect E Struct Rep Online. 2008 September 1; 64(Pt 9): m1146–m1147.
Published online 2008 August 9. doi:  10.1107/S1600536808024525
PMCID: PMC2960491

{μ-N-[(Diphenyl­phosphino)meth­yl]pyridin-2-amine-κ2 N 1:P}bis­{[2-(2,2′-bipyridin-6-yl)phenyl-κ3 N,N′,C 1]platinum(II)} bis­(perchlorate)

Abstract

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 [triangle]); Catalano et al. (2001 [triangle]); Durran et al. (2000 [triangle]); Field et al. (1997 [triangle]); Kuang et al. (1998 [triangle]); Li et al. (1996 [triangle]); Newkome (1993 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1146-scheme1.jpg

Experimental

Crystal data

  • [Pt2(C16H11N2)2(C18H17N2P)](ClO4)2
  • M r = 1343.92
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1146-efi1.jpg
  • a = 14.845 (3) Å
  • b = 17.927 (4) Å
  • c = 18.481 (4) Å
  • β = 109.697 (3)°
  • V = 4630.5 (18) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 6.25 mm−1
  • T = 294 (2) K
  • 0.40 × 0.20 × 0.10 mm

Data collection

  • Bruker SMART APEX CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.225, T max = 0.533
  • 22850 measured reflections
  • 8097 independent reflections
  • 5253 reflections with I > 2σ(I)
  • R int = 0.090

Refinement

  • R[F 2 > 2σ(F 2)] = 0.075
  • wR(F 2) = 0.219
  • S = 1.03
  • 8097 reflections
  • 696 parameters
  • 16 restraints
  • H-atom parameters constrained
  • Δρmax = 2.85 e Å−3
  • Δρmin = −2.38 e Å−3

Data collection: SMART (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808024525/hy2138sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808024525/hy2138Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank Henan Agricultural University for the generous support of this study.

supplementary crystallographic information

Comment

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)°.

Experimental

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.

Refinement

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.

Figures

Fig. 1.
Molecular structure of the title compound. Displacement ellipsoids are drawn at the 40% probability level. H atoms and the minor disordered positions of the perchlorate anions have been omitted for clarity.

Crystal data

[Pt2(C16H11N2)2(C18H17N2P)](ClO4)2F000 = 2600
Mr = 1343.92Dx = 1.928 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7716 reflections
a = 14.845 (3) Åθ = 2.3–26.6º
b = 17.927 (4) ŵ = 6.25 mm1
c = 18.481 (4) ÅT = 294 (2) K
β = 109.697 (3)ºBlock, yellow
V = 4630.5 (18) Å30.40 × 0.20 × 0.10 mm
Z = 4

Data collection

Bruker SMART APEX CCD area-detector diffractometer8097 independent reflections
Radiation source: fine-focus sealed tube5253 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.090
T = 294(2) Kθmax = 25.0º
[var phi] and ω scansθmin = 1.6º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −17→16
Tmin = 0.225, Tmax = 0.534k = −17→21
22850 measured reflectionsl = −20→21

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.075H-atom parameters constrained
wR(F2) = 0.219  w = 1/[σ2(Fo2) + (0.0656P)2 + 39.0816P] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
8097 reflectionsΔρmax = 2.85 e Å3
696 parametersΔρmin = −2.38 e Å3
16 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Pt10.96899 (4)0.15372 (3)0.47609 (3)0.0324 (2)
Pt20.71657 (4)0.21672 (3)0.51620 (3)0.0326 (2)
P10.7571 (3)0.3339 (2)0.55627 (19)0.0325 (8)
N10.9510 (9)0.1645 (8)0.3600 (6)0.040 (3)
N20.8943 (8)0.0657 (8)0.4355 (6)0.033 (3)
N31.0503 (9)0.2462 (8)0.5165 (5)0.038 (3)
N40.9260 (9)0.3020 (8)0.5450 (7)0.040 (3)
H40.90290.25820.54640.048*
N50.7113 (10)0.1553 (8)0.6155 (8)0.047 (3)
N60.6669 (8)0.1175 (7)0.4717 (7)0.033 (3)
C10.9763 (13)0.2199 (10)0.3226 (9)0.047 (4)
H11.00690.26130.35040.056*
C20.9588 (14)0.2184 (12)0.2437 (10)0.060 (5)
H20.97810.25790.21980.072*
C30.9137 (15)0.1595 (13)0.2027 (9)0.065 (6)
H30.90370.15720.15030.078*
C40.8816 (12)0.1013 (11)0.2385 (9)0.053 (5)
H4A0.84770.06160.20950.064*
C50.9009 (11)0.1032 (9)0.3175 (8)0.040 (4)
C60.8704 (10)0.0466 (10)0.3612 (7)0.039 (4)
C70.8170 (11)−0.0157 (11)0.3327 (9)0.053 (5)
H70.7987−0.02680.28060.063*
C80.7905 (12)−0.0622 (11)0.3821 (10)0.056 (5)
H80.7547−0.10500.36380.068*
C90.8179 (10)−0.0437 (10)0.4582 (9)0.042 (4)
H90.7979−0.07330.49120.050*
C100.8741 (10)0.0176 (9)0.4873 (7)0.034 (3)
C110.9076 (10)0.0489 (9)0.5636 (8)0.035 (3)
C120.8939 (11)0.0107 (11)0.6275 (8)0.047 (4)
H120.8600−0.03380.62030.056*
C130.9321 (14)0.0416 (13)0.6992 (9)0.063 (5)
H130.92260.01820.74090.076*
C140.9833 (13)0.1055 (13)0.7101 (9)0.061 (5)
H141.01030.12420.75970.073*
C150.9969 (12)0.1443 (10)0.6490 (8)0.045 (4)
H151.02980.18940.65800.054*
C160.9616 (9)0.1158 (11)0.5751 (7)0.042 (4)
C171.1411 (10)0.2502 (11)0.5117 (9)0.044 (4)
H171.16490.20900.49330.053*
C181.1961 (13)0.3111 (10)0.5326 (10)0.049 (4)
H181.25810.31030.53110.059*
C191.1611 (10)0.3767 (10)0.5568 (8)0.041 (4)
H191.19700.42030.56810.049*
C201.0709 (11)0.3726 (9)0.5628 (7)0.039 (4)
H201.04640.41310.58140.047*
C211.0161 (10)0.3071 (9)0.5406 (6)0.030 (3)
C220.8681 (9)0.3651 (9)0.5475 (8)0.034 (3)
H22A0.85540.39430.50090.041*
H22B0.90180.39650.59090.041*
C230.7700 (12)0.3500 (8)0.6562 (8)0.040 (4)
C240.8588 (12)0.3455 (11)0.7132 (9)0.054 (5)
H240.91410.34320.70030.065*
C250.8646 (16)0.3446 (13)0.7892 (10)0.077 (7)
H250.92420.33900.82710.092*
C260.7854 (14)0.3515 (12)0.8103 (10)0.059 (5)
H260.79020.35140.86180.070*
C270.6987 (15)0.3588 (12)0.7532 (9)0.064 (6)
H270.64400.36350.76660.077*
C280.6894 (13)0.3592 (12)0.6757 (9)0.055 (5)
H280.62980.36560.63800.067*
C290.6740 (10)0.4050 (9)0.5055 (7)0.035 (3)
C300.5850 (11)0.3829 (11)0.4536 (7)0.043 (4)
H300.56890.33280.44500.051*
C310.5226 (16)0.4377 (15)0.4159 (10)0.074 (7)
H310.46370.42390.38070.089*
C320.5421 (17)0.5077 (13)0.4274 (12)0.072 (7)
H320.49660.54320.40220.086*
C330.6317 (15)0.5307 (12)0.4777 (13)0.069 (6)
H330.64620.58130.48420.083*
C340.6956 (13)0.4806 (10)0.5160 (10)0.048 (4)
H340.75470.49590.54980.058*
C350.7382 (16)0.1770 (13)0.6886 (10)0.067 (6)
H350.76500.22410.70190.080*
C360.7269 (18)0.1308 (15)0.7452 (13)0.081 (7)
H360.75040.14580.79630.097*
C370.6828 (16)0.0650 (16)0.7270 (13)0.085 (8)
H370.66920.03610.76380.102*
C380.6578 (15)0.0413 (13)0.6510 (12)0.070 (6)
H380.6328−0.00620.63750.084*
C390.6702 (11)0.0888 (9)0.5949 (9)0.044 (4)
C400.6436 (12)0.0660 (11)0.5145 (11)0.055 (5)
C410.6049 (13)−0.0013 (11)0.4835 (11)0.059 (5)
H410.5944−0.03830.51510.070*
C420.5824 (13)−0.0137 (12)0.4087 (13)0.065 (6)
H420.5563−0.05910.38750.078*
C430.5988 (13)0.0432 (12)0.3620 (12)0.066 (6)
H430.58050.03660.30910.079*
C440.6428 (10)0.1095 (10)0.3956 (9)0.042 (4)
C450.6726 (11)0.1717 (10)0.3581 (8)0.038 (4)
C460.6645 (13)0.1717 (12)0.2834 (9)0.056 (5)
H460.63590.13160.25230.068*
C470.6988 (14)0.2316 (14)0.2526 (9)0.067 (6)
H470.69760.23000.20190.081*
C480.7345 (13)0.2930 (12)0.2973 (9)0.060 (5)
H480.75580.33390.27650.072*
C490.7389 (12)0.2942 (11)0.3716 (8)0.049 (4)
H490.76120.33740.39990.059*
C500.7124 (10)0.2355 (9)0.4077 (7)0.034 (4)
Cl10.9289 (4)0.2821 (3)0.0174 (3)0.0685 (14)
Cl20.4595 (5)0.0612 (3)0.8325 (2)0.0868 (19)
O10.8360 (8)0.3152 (11)0.0026 (12)0.045 (7)0.49 (3)
O20.9880 (13)0.3037 (16)0.0961 (7)0.085 (11)0.49 (3)
O30.9732 (14)0.3115 (14)−0.0339 (11)0.066 (10)0.49 (3)
O40.9225 (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)
O50.5418 (15)0.0136 (14)0.8519 (16)0.126 (14)0.52 (2)
O60.465 (2)0.1108 (12)0.8945 (10)0.089 (10)0.52 (2)
O70.452 (2)0.1028 (12)0.7643 (9)0.070 (9)0.52 (2)
O80.3747 (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)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pt10.0415 (4)0.0279 (4)0.0241 (3)0.0019 (2)0.0060 (2)−0.0019 (2)
Pt20.0420 (4)0.0225 (4)0.0301 (3)−0.0007 (2)0.0079 (2)−0.0017 (2)
P10.044 (2)0.025 (2)0.0253 (17)0.0033 (17)0.0066 (14)−0.0016 (14)
N10.057 (8)0.037 (9)0.030 (6)−0.001 (7)0.021 (6)−0.006 (5)
N20.035 (7)0.039 (8)0.020 (5)−0.002 (6)0.003 (4)0.002 (5)
N30.048 (7)0.049 (9)0.013 (5)0.001 (7)0.004 (5)−0.001 (5)
N40.046 (8)0.034 (8)0.044 (7)−0.011 (6)0.021 (6)−0.007 (6)
N50.046 (8)0.033 (9)0.059 (9)0.000 (6)0.012 (6)0.006 (6)
N60.030 (7)0.026 (7)0.044 (7)0.009 (5)0.014 (5)−0.007 (5)
C10.066 (11)0.035 (11)0.040 (8)−0.002 (9)0.019 (7)0.003 (7)
C20.078 (13)0.064 (16)0.047 (10)0.018 (11)0.032 (9)0.021 (9)
C30.087 (14)0.078 (17)0.026 (8)0.003 (12)0.014 (8)−0.005 (9)
C40.066 (11)0.042 (12)0.041 (9)0.015 (9)0.003 (7)−0.006 (8)
C50.052 (9)0.029 (9)0.034 (7)0.017 (8)0.009 (6)−0.002 (6)
C60.040 (8)0.047 (11)0.027 (7)0.018 (8)0.006 (6)−0.006 (6)
C70.050 (10)0.055 (13)0.041 (9)0.004 (9)−0.001 (7)−0.016 (8)
C80.060 (11)0.037 (11)0.059 (11)−0.012 (9)0.004 (8)−0.019 (8)
C90.037 (8)0.033 (10)0.063 (10)−0.002 (7)0.025 (7)0.005 (7)
C100.044 (8)0.023 (8)0.034 (7)0.003 (7)0.011 (6)0.006 (6)
C110.035 (8)0.033 (9)0.035 (7)0.005 (7)0.008 (6)0.006 (6)
C120.043 (9)0.054 (12)0.041 (8)0.001 (8)0.010 (7)0.013 (8)
C130.082 (13)0.074 (16)0.034 (9)0.002 (12)0.020 (8)0.015 (9)
C140.075 (13)0.078 (17)0.028 (8)−0.007 (12)0.013 (7)−0.003 (8)
C150.061 (10)0.043 (11)0.026 (7)−0.002 (8)0.009 (7)0.003 (6)
C160.017 (7)0.079 (14)0.026 (7)0.000 (8)0.002 (5)−0.015 (7)
C170.035 (9)0.052 (12)0.059 (9)0.011 (8)0.033 (7)0.011 (8)
C180.055 (10)0.027 (10)0.063 (10)−0.002 (8)0.015 (8)0.004 (7)
C190.031 (8)0.043 (11)0.043 (8)−0.020 (7)0.006 (6)−0.001 (7)
C200.059 (10)0.023 (9)0.027 (7)−0.013 (7)0.002 (6)−0.004 (6)
C210.039 (8)0.034 (9)0.015 (6)0.001 (7)0.005 (5)−0.010 (5)
C220.031 (8)0.046 (10)0.028 (7)0.004 (7)0.013 (6)−0.002 (6)
C230.069 (11)0.012 (8)0.033 (7)0.003 (7)0.008 (7)−0.010 (5)
C240.050 (10)0.068 (15)0.039 (9)−0.005 (9)0.009 (7)0.000 (8)
C250.095 (16)0.085 (19)0.029 (9)−0.025 (13)−0.007 (9)−0.012 (9)
C260.079 (14)0.062 (15)0.037 (9)−0.010 (11)0.022 (9)−0.016 (8)
C270.094 (15)0.067 (16)0.037 (9)0.004 (11)0.031 (9)−0.007 (8)
C280.062 (11)0.064 (14)0.040 (9)0.031 (10)0.017 (8)0.011 (8)
C290.041 (8)0.033 (10)0.028 (7)0.016 (7)0.009 (6)0.003 (6)
C300.053 (10)0.051 (12)0.021 (7)0.013 (8)0.008 (6)−0.004 (6)
C310.092 (15)0.09 (2)0.035 (9)0.043 (14)0.015 (9)0.016 (10)
C320.098 (17)0.050 (15)0.083 (14)0.053 (13)0.050 (13)0.046 (11)
C330.084 (15)0.048 (15)0.096 (15)0.008 (12)0.058 (13)0.039 (12)
C340.066 (11)0.031 (11)0.063 (10)0.018 (8)0.042 (9)0.016 (8)
C350.111 (16)0.051 (13)0.036 (9)0.010 (12)0.021 (9)0.015 (8)
C360.123 (19)0.067 (17)0.065 (13)−0.010 (15)0.048 (13)0.026 (11)
C370.094 (16)0.09 (2)0.083 (16)0.003 (14)0.044 (13)0.055 (14)
C380.092 (15)0.041 (13)0.081 (14)−0.008 (11)0.034 (11)0.006 (10)
C390.046 (9)0.024 (9)0.063 (10)0.002 (7)0.020 (7)0.000 (7)
C400.047 (10)0.033 (11)0.070 (11)−0.004 (8)0.001 (8)−0.015 (9)
C410.068 (12)0.028 (11)0.075 (12)0.014 (9)0.018 (9)−0.003 (9)
C420.049 (11)0.039 (13)0.106 (16)−0.006 (9)0.022 (10)−0.020 (11)
C430.058 (11)0.044 (13)0.074 (12)−0.003 (10)−0.007 (9)−0.037 (10)
C440.027 (8)0.044 (11)0.048 (9)0.007 (7)0.005 (6)−0.009 (7)
C450.041 (9)0.036 (10)0.026 (7)0.007 (7)−0.002 (6)−0.003 (6)
C460.069 (12)0.051 (13)0.029 (8)0.026 (10)−0.010 (7)−0.013 (8)
C470.084 (14)0.083 (18)0.026 (8)0.039 (13)0.007 (8)0.007 (9)
C480.071 (12)0.053 (13)0.043 (9)0.020 (10)0.004 (8)0.006 (8)
C490.065 (11)0.050 (12)0.026 (7)−0.016 (9)0.006 (7)0.001 (7)
C500.034 (8)0.040 (10)0.030 (7)0.008 (7)0.012 (6)−0.020 (6)
Cl10.070 (3)0.057 (4)0.091 (4)0.007 (3)0.044 (3)0.023 (3)
Cl20.158 (6)0.043 (3)0.038 (2)0.008 (3)0.005 (3)0.000 (2)
O10.043 (10)0.049 (11)0.046 (10)−0.003 (8)0.021 (7)−0.006 (7)
O20.092 (13)0.083 (14)0.076 (13)0.002 (9)0.022 (9)0.009 (9)
O30.071 (12)0.066 (13)0.059 (12)−0.008 (9)0.021 (8)−0.007 (9)
O40.099 (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)
O50.123 (16)0.120 (17)0.129 (16)0.006 (10)0.034 (10)0.009 (10)
O60.100 (13)0.085 (13)0.073 (12)−0.003 (9)0.018 (8)−0.013 (9)
O70.081 (12)0.055 (12)0.067 (11)−0.005 (9)0.018 (8)0.012 (8)
O80.153 (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)

Geometric parameters (Å, °)

Pt1—N21.928 (13)C24—C251.38 (2)
Pt1—C161.990 (15)C24—H240.9300
Pt1—N32.038 (14)C25—C261.36 (3)
Pt1—N12.079 (11)C25—H250.9300
Pt2—N61.993 (13)C26—C271.37 (3)
Pt2—C502.014 (14)C26—H260.9300
Pt2—N52.164 (14)C27—C281.39 (2)
Pt2—P12.241 (4)C27—H270.9300
P1—C221.799 (14)C28—H280.9300
P1—C291.802 (14)C29—C341.39 (2)
P1—C231.814 (14)C29—C301.40 (2)
N1—C11.34 (2)C30—C311.37 (3)
N1—C51.41 (2)C30—H300.9300
N2—C61.342 (17)C31—C321.29 (3)
N2—C101.394 (18)C31—H310.9300
N3—C211.342 (19)C32—C331.40 (3)
N3—C171.381 (19)C32—H320.9300
N4—C211.370 (18)C33—C341.33 (2)
N4—C221.43 (2)C33—H330.9300
N4—H40.8600C34—H340.9300
N5—C351.33 (2)C35—C361.39 (3)
N5—C391.34 (2)C35—H350.9300
N6—C401.33 (2)C36—C371.34 (4)
N6—C441.338 (19)C36—H360.9300
C1—C21.39 (2)C37—C381.39 (3)
C1—H10.9300C37—H370.9300
C2—C31.34 (3)C38—C391.40 (3)
C2—H20.9300C38—H380.9300
C3—C41.40 (3)C39—C401.46 (2)
C3—H30.9300C40—C411.38 (3)
C4—C51.39 (2)C41—C421.33 (3)
C4—H4A0.9300C41—H410.9300
C5—C61.46 (2)C42—C431.41 (3)
C6—C71.37 (2)C42—H420.9300
C7—C81.39 (3)C43—C441.40 (2)
C7—H70.9300C43—H430.9300
C8—C91.37 (2)C44—C451.46 (2)
C8—H80.9300C45—C461.35 (2)
C9—C101.37 (2)C45—C501.46 (2)
C9—H90.9300C46—C471.39 (3)
C10—C111.44 (2)C46—H460.9300
C11—C161.42 (2)C47—C481.37 (3)
C11—C121.44 (2)C47—H470.9300
C12—C131.37 (2)C48—C491.35 (2)
C12—H120.9300C48—H480.9300
C13—C141.35 (3)C49—C501.37 (2)
C13—H130.9300C49—H490.9300
C14—C151.40 (2)Cl1—O41.421 (8)
C14—H140.9300Cl1—O31.424 (8)
C15—C161.39 (2)Cl1—O3'1.427 (8)
C15—H150.9300Cl1—O2'1.432 (8)
C17—C181.34 (2)Cl1—O1'1.434 (8)
C17—H170.9300Cl1—O11.440 (8)
C18—C191.42 (3)Cl1—O4'1.461 (9)
C18—H180.9300Cl1—O21.474 (8)
C19—C201.38 (2)Cl2—O61.430 (9)
C19—H190.9300Cl2—O7'1.431 (8)
C20—C211.41 (2)Cl2—O5'1.434 (8)
C20—H200.9300Cl2—O51.435 (9)
C22—H22A0.9700Cl2—O71.437 (8)
C22—H22B0.9700Cl2—O8'1.439 (9)
C23—C281.37 (2)Cl2—O6'1.452 (9)
C23—C241.39 (2)Cl2—O81.453 (9)
N2—Pt1—C1682.8 (6)C23—C28—H28120.8
N2—Pt1—N3178.1 (4)C27—C28—H28120.8
C16—Pt1—N398.7 (6)C34—C29—C30119.3 (14)
N2—Pt1—N179.5 (5)C34—C29—P1122.1 (12)
C16—Pt1—N1162.3 (6)C30—C29—P1118.6 (13)
N3—Pt1—N199.0 (5)C31—C30—C29118 (2)
N6—Pt2—C5081.7 (6)C31—C30—H30121.1
N6—Pt2—N577.4 (5)C29—C30—H30121.1
C50—Pt2—N5158.8 (6)C32—C31—C30123 (2)
N6—Pt2—P1173.4 (4)C32—C31—H31118.7
C50—Pt2—P195.0 (5)C30—C31—H31118.7
N5—Pt2—P1106.2 (4)C31—C32—C33120.4 (18)
C22—P1—C29102.7 (7)C31—C32—H32119.8
C22—P1—C23104.9 (7)C33—C32—H32119.8
C29—P1—C23103.7 (7)C34—C33—C32120 (2)
C22—P1—Pt2114.5 (5)C34—C33—H33119.9
C29—P1—Pt2115.5 (5)C32—C33—H33119.9
C23—P1—Pt2114.2 (5)C33—C34—C29119.7 (19)
C1—N1—C5118.6 (13)C33—C34—H34120.1
C1—N1—Pt1130.0 (12)C29—C34—H34120.1
C5—N1—Pt1111.3 (10)N5—C35—C36121 (2)
C6—N2—C10120.0 (14)N5—C35—H35119.4
C6—N2—Pt1121.8 (11)C36—C35—H35119.4
C10—N2—Pt1117.9 (9)C37—C36—C35121 (2)
C21—N3—C17117.7 (15)C37—C36—H36119.6
C21—N3—Pt1122.7 (10)C35—C36—H36119.6
C17—N3—Pt1119.3 (12)C36—C37—C38117.7 (17)
C21—N4—C22123.9 (14)C36—C37—H37121.2
C21—N4—H4118.1C38—C37—H37121.2
C22—N4—H4118.1C37—C38—C39120 (2)
C35—N5—C39120.2 (15)C37—C38—H38119.9
C35—N5—Pt2128.9 (13)C39—C38—H38119.9
C39—N5—Pt2110.8 (11)N5—C39—C38119.5 (16)
C40—N6—C44121.2 (15)N5—C39—C40118.8 (15)
C40—N6—Pt2120.5 (11)C38—C39—C40121.7 (17)
C44—N6—Pt2117.4 (11)N6—C40—C41121.1 (18)
N1—C1—C2122.9 (18)N6—C40—C39111.9 (15)
N1—C1—H1118.6C41—C40—C39126.9 (19)
C2—C1—H1118.6C42—C41—C40120 (2)
C3—C2—C1119.2 (18)C42—C41—H41119.9
C3—C2—H2120.4C40—C41—H41119.9
C1—C2—H2120.4C41—C42—C43118.9 (19)
C2—C3—C4120.3 (16)C41—C42—H42120.6
C2—C3—H3119.9C43—C42—H42120.6
C4—C3—H3119.9C44—C43—C42119.6 (18)
C5—C4—C3119.6 (18)C44—C43—H43120.2
C5—C4—H4A120.2C42—C43—H43120.2
C3—C4—H4A120.2N6—C44—C43118.6 (17)
C4—C5—N1119.2 (16)N6—C44—C45113.6 (15)
C4—C5—C6124.8 (16)C43—C44—C45127.7 (16)
N1—C5—C6115.9 (12)C46—C45—C44123.5 (17)
N2—C6—C7121.5 (15)C46—C45—C50121.4 (17)
N2—C6—C5111.3 (15)C44—C45—C50115.2 (13)
C7—C6—C5127.0 (13)C45—C46—C47120.2 (18)
C6—C7—C8119.5 (15)C45—C46—H46119.9
C6—C7—H7120.2C47—C46—H46119.9
C8—C7—H7120.2C48—C47—C46119.6 (17)
C9—C8—C7118.6 (16)C48—C47—H47120.2
C9—C8—H8120.7C46—C47—H47120.2
C7—C8—H8120.7C49—C48—C47120 (2)
C8—C9—C10121.8 (15)C49—C48—H48119.9
C8—C9—H9119.1C47—C48—H48119.9
C10—C9—H9119.1C48—C49—C50123.8 (18)
C9—C10—N2117.9 (12)C48—C49—H49118.1
C9—C10—C11131.1 (13)C50—C49—H49118.1
N2—C10—C11110.3 (13)C49—C50—C45114.7 (13)
C16—C11—C12120.6 (13)C49—C50—Pt2134.0 (12)
C16—C11—C10117.9 (12)C45—C50—Pt2111.3 (12)
C12—C11—C10121.3 (15)O4—Cl1—O3112.5 (8)
C13—C12—C11118.4 (17)O4—Cl1—O3'134.0 (12)
C13—C12—H12120.8O4—Cl1—O2'62.8 (14)
C11—C12—H12120.8O3—Cl1—O2'112.1 (14)
C14—C13—C12121.0 (16)O3'—Cl1—O2'111.2 (8)
C14—C13—H13119.5O4—Cl1—O1'114.2 (13)
C12—C13—H13119.5O3—Cl1—O1'127.1 (13)
C13—C14—C15121.8 (15)O3'—Cl1—O1'110.3 (8)
C13—C14—H14119.1O2'—Cl1—O1'110.3 (8)
C15—C14—H14119.1O4—Cl1—O1110.9 (8)
C16—C15—C14120.3 (17)O3—Cl1—O1110.4 (8)
C16—C15—H15119.9O3'—Cl1—O1102.8 (13)
C14—C15—H15119.9O2'—Cl1—O1135.7 (12)
C15—C16—C11117.8 (14)O4—Cl1—O4'46.4 (13)
C15—C16—Pt1131.4 (14)O3—Cl1—O4'86.9 (13)
C11—C16—Pt1110.7 (9)O3'—Cl1—O4'108.4 (8)
C18—C17—N3122.5 (17)O2'—Cl1—O4'108.0 (8)
C18—C17—H17118.8O1'—Cl1—O4'108.5 (8)
N3—C17—H17118.8O1—Cl1—O4'86.3 (12)
C17—C18—C19120.9 (17)O4—Cl1—O2108.1 (8)
C17—C18—H18119.5O3—Cl1—O2107.8 (8)
C19—C18—H18119.5O3'—Cl1—O290.2 (12)
C20—C19—C18116.7 (16)O2'—Cl1—O247.4 (13)
C20—C19—H19121.6O1'—Cl1—O279.8 (12)
C18—C19—H19121.6O1—Cl1—O2107.0 (7)
C19—C20—C21120.1 (15)O4'—Cl1—O2154.4 (13)
C19—C20—H20120.0O6—Cl2—O7'111.9 (14)
C21—C20—H20120.0O6—Cl2—O5'137.2 (13)
N3—C21—N4116.8 (14)O7'—Cl2—O5'110.9 (8)
N3—C21—C20122.0 (14)O6—Cl2—O5110.9 (8)
N4—C21—C20121.2 (14)O7'—Cl2—O5129.3 (14)
N4—C22—P1109.6 (11)O6—Cl2—O7110.4 (8)
N4—C22—H22A109.8O5'—Cl2—O7107.4 (14)
P1—C22—H22A109.8O5—Cl2—O7109.5 (8)
N4—C22—H22B109.8O6—Cl2—O8'53.3 (14)
P1—C22—H22B109.8O7'—Cl2—O8'110.0 (8)
H22A—C22—H22B108.2O5'—Cl2—O8'109.9 (8)
C28—C23—C24119.8 (14)O5—Cl2—O8'116.9 (15)
C28—C23—P1119.0 (12)O7—Cl2—O8'133.6 (14)
C24—C23—P1120.8 (13)O6—Cl2—O6'57.0 (13)
C25—C24—C23119.6 (17)O7'—Cl2—O6'109.1 (8)
C25—C24—H24120.2O5'—Cl2—O6'108.7 (8)
C23—C24—H24120.2O5—Cl2—O6'73.9 (14)
C26—C25—C24121.8 (18)O7—Cl2—O6'84.2 (13)
C26—C25—H25119.1O8'—Cl2—O6'108.3 (8)
C24—C25—H25119.1O6—Cl2—O8108.4 (8)
C25—C26—C27117.7 (16)O7'—Cl2—O882.0 (12)
C25—C26—H26121.2O5'—Cl2—O876.8 (14)
C27—C26—H26121.2O5—Cl2—O8108.6 (8)
C26—C27—C28122.5 (18)O7—Cl2—O8109.0 (8)
C26—C27—H27118.8O8'—Cl2—O855.9 (14)
C28—C27—H27118.8O6'—Cl2—O8163.8 (14)
C23—C28—C27118.5 (16)
C50—Pt2—P1—C22−59.8 (6)Pt1—N3—C21—C20−175.0 (9)
N5—Pt2—P1—C22118.4 (6)C22—N4—C21—N3−161.1 (12)
C50—Pt2—P1—C2959.2 (6)C22—N4—C21—C2020.9 (19)
N5—Pt2—P1—C29−122.6 (6)C19—C20—C21—N33(2)
C50—Pt2—P1—C23179.3 (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—C1174.6 (16)C29—P1—C22—N4−148.3 (9)
C16—Pt1—N1—C1173.0 (18)C23—P1—C22—N4103.6 (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—C28155.5 (14)
C16—Pt1—N1—C5−4(2)C29—P1—C23—C2848.1 (16)
N3—Pt1—N1—C5176.0 (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—C64.4 (11)C29—P1—C23—C24−138.5 (14)
C16—Pt1—N2—C10−2.9 (11)Pt2—P1—C23—C2495.0 (14)
N1—Pt1—N2—C10177.6 (11)C28—C23—C24—C255(3)
C16—Pt1—N3—C21−72.3 (11)P1—C23—C24—C25−168.3 (16)
N1—Pt1—N3—C21107.6 (11)C23—C24—C25—C26−3(3)
C16—Pt1—N3—C17114.7 (11)C24—C25—C26—C271(3)
N1—Pt1—N3—C17−65.4 (11)C25—C26—C27—C280(3)
N6—Pt2—N5—C35177.4 (17)C24—C23—C28—C27−4(3)
C50—Pt2—N5—C35166.7 (16)P1—C23—C28—C27169.1 (16)
P1—Pt2—N5—C35−8.3 (17)C26—C27—C28—C232(3)
N6—Pt2—N5—C39−6.1 (11)C22—P1—C29—C34−45.2 (13)
C50—Pt2—N5—C39−17 (2)C23—P1—C29—C3463.8 (13)
P1—Pt2—N5—C39168.1 (10)Pt2—P1—C29—C34−170.5 (10)
C50—Pt2—N6—C40−176.6 (13)C22—P1—C29—C30134.6 (11)
N5—Pt2—N6—C407.4 (12)C23—P1—C29—C30−116.4 (12)
C50—Pt2—N6—C44−7.6 (10)Pt2—P1—C29—C309.3 (12)
N5—Pt2—N6—C44176.3 (11)C34—C29—C30—C31−1(2)
C5—N1—C1—C2−3(3)P1—C29—C30—C31179.5 (12)
Pt1—N1—C1—C2−180.0 (13)C29—C30—C31—C32−1(3)
N1—C1—C2—C31(3)C30—C31—C32—C333(3)
C1—C2—C3—C42(3)C31—C32—C33—C34−3(3)
C2—C3—C4—C5−3(3)C32—C33—C34—C291(2)
C3—C4—C5—N11(2)C30—C29—C34—C331(2)
C3—C4—C5—C6179.2 (16)P1—C29—C34—C33−179.5 (12)
C1—N1—C5—C42(2)C39—N5—C35—C362(3)
Pt1—N1—C5—C4179.5 (12)Pt2—N5—C35—C36178.0 (16)
C1—N1—C5—C6−176.5 (14)N5—C35—C36—C37−5(4)
Pt1—N1—C5—C61.3 (16)C35—C36—C37—C387(4)
C10—N2—C6—C77(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—C404.7 (19)
N1—C5—C6—N21.9 (19)C37—C38—C39—N54(3)
C4—C5—C6—C7−2(3)C37—C38—C39—C40−179.3 (18)
N1—C5—C6—C7176.5 (15)C44—N6—C40—C418(3)
N2—C6—C7—C8−3(2)Pt2—N6—C40—C41176.8 (13)
C5—C6—C7—C8−177.0 (16)C44—N6—C40—C39−175.5 (13)
C6—C7—C8—C91(3)Pt2—N6—C40—C39−6.9 (19)
C7—C8—C9—C10−3(3)N5—C39—C40—N61(2)
C8—C9—C10—N27(2)C38—C39—C40—N6−176.0 (16)
C8—C9—C10—C11177.0 (17)N5—C39—C40—C41176.8 (17)
C6—N2—C10—C9−9(2)C38—C39—C40—C410(3)
Pt1—N2—C10—C9177.6 (11)N6—C40—C41—C42−6(3)
C6—N2—C10—C11179.0 (12)C39—C40—C41—C42178.6 (18)
Pt1—N2—C10—C115.6 (16)C40—C41—C42—C430(3)
C9—C10—C11—C16−176.9 (16)C41—C42—C43—C443(3)
N2—C10—C11—C16−6.3 (19)C40—N6—C44—C43−5(2)
C9—C10—C11—C128(3)Pt2—N6—C44—C43−173.6 (12)
N2—C10—C11—C12178.9 (13)C40—N6—C44—C45179.0 (14)
C16—C11—C12—C132(2)Pt2—N6—C44—C4510.1 (17)
C10—C11—C12—C13176.4 (16)C42—C43—C44—N6−1(3)
C11—C12—C13—C14−2(3)C42—C43—C44—C45174.6 (17)
C12—C13—C14—C152(3)N6—C44—C45—C46172.9 (14)
C13—C14—C15—C16−3(3)C43—C44—C45—C46−3(3)
C14—C15—C16—C113(2)N6—C44—C45—C50−7(2)
C14—C15—C16—Pt1−178.8 (13)C43—C44—C45—C50176.9 (15)
C12—C11—C16—C15−3(2)C44—C45—C46—C47−176.8 (16)
C10—C11—C16—C15−177.5 (14)C50—C45—C46—C473(3)
C12—C11—C16—Pt1179.0 (11)C45—C46—C47—C48−5(3)
C10—C11—C16—Pt14.1 (17)C46—C47—C48—C492(3)
N2—Pt1—C16—C15−178.8 (16)C47—C48—C49—C502(3)
N3—Pt1—C16—C152.4 (17)C48—C49—C50—C45−4(2)
N1—Pt1—C16—C15−177.2 (15)C48—C49—C50—Pt2176.0 (13)
N2—Pt1—C16—C11−0.7 (11)C46—C45—C50—C491(2)
N3—Pt1—C16—C11−179.5 (10)C44—C45—C50—C49−179.1 (14)
N1—Pt1—C16—C111(3)C46—C45—C50—Pt2−179.0 (12)
C21—N3—C17—C182(2)C44—C45—C50—Pt21.2 (16)
Pt1—N3—C17—C18175.7 (12)N6—Pt2—C50—C49−176.6 (17)
N3—C17—C18—C19−4(2)N5—Pt2—C50—C49−165.9 (15)
C17—C18—C19—C204(2)P1—Pt2—C50—C499.2 (16)
C18—C19—C20—C21−4(2)N6—Pt2—C50—C453.1 (10)
C17—N3—C21—N4−179.9 (12)N5—Pt2—C50—C4514 (2)
Pt1—N3—C21—N46.9 (16)P1—Pt2—C50—C45−171.1 (9)
C17—N3—C21—C20−1.9 (19)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2138).

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