Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680703070X/ng2287sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680703070X/ng2287Isup2.hkl |
CCDC reference: 657512
(2,2':6',2''-Terpyridyl-κ3N)dinitratopalladium (46.4 mg, 0.10 mmol) was dissolved in water (5 ml), and a tenfold excess of potassium hexafluorophosphate was added, which resulted in the immediate deposition deep yellow microcrystals. The crystals were filtered, washed with a minimum amount of cold water and dried under vacuum (quantative yield of 59.6 mg). Crystals were obtained by the vapor diffusion of diethyl ether into a 2 mM solution in acetonitrile.
The aromatic H atoms were constrained to an ideal geometry, with C—H distances of 0.93 Å and Uiso(H) = 1.2Ueq(C). The methyl H atoms were rotated to fit the electron density, with C—H distances of 0.96 Å and Uiso(H) = 1.5Ueq(C). The largest peak and deepest hole on the final difference Fourier map corresponds to 0.84 and -0.61 e.Å-3, and were located 1.14 and 0.42Å from the F12 and F10 atoms.
The 2,2':6',2''-terpyridine complexes of palladium(II) and platinum(II) have the metal centers in a square-planar geometry (Angle et al., 2006; Onoda et al., 2003; Roszak et al., 1996). The title compound also displays square-planar coordination, with four N atoms from terpy and acetonitrile molecule (Fig. 1). The crystal structure comprises alternating layers of cations and anions as represented in Fig. 2. The compound packs by an anion–π interaction (P1—F2···Cg1 3.063 (5) Å [Cg1 is the centroid of the ring system Pd1, N1, C5, C6, N2; P2—F12···Cg2 3.076 (6) Å, Cg2 is the centroid of the ring system Pd1, N2, C10, C11, N3] and hydrogen bonds involving hexafluorophosphate anions (C—H···F). Non-classical hydrogen bonds that connect cations, anions and coordinated acetonitrile molecules are detailed in Table 2.
For literature on the 2,2':6',2''-terpyridine complexes of palladium(II) and platinum(II), see: Angle et al. (2006); Onoda et al. (2003); Roszak et al. (1996).
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. A view of the title compound (I), showing 30% probability displacement ellipsoids and the atom numbering scheme. |
[Pd(C15H11N3)(C2H3N)](PF6)2 | F(000) = 1312 |
Mr = 670.66 | Dx = 1.976 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8518 reflections |
a = 13.1073 (3) Å | θ = 2.2–28.3° |
b = 11.8840 (3) Å | µ = 1.08 mm−1 |
c = 14.6085 (4) Å | T = 273 K |
β = 97.810 (1)° | Block, yellow |
V = 2254.42 (10) Å3 | 0.30 × 0.24 × 0.22 mm |
Z = 4 |
Bruker SMART diffractometer | 5449 independent reflections |
Radiation source: sealed tube | 4503 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
φ and ω scans | θmax = 28.3°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −15→17 |
Tmin = 0.738, Tmax = 0.797 | k = −15→15 |
16715 measured reflections | l = −19→18 |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.142 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0789P)2 + 2.9852P] where P = (Fo2 + 2Fc2)/3 |
5449 reflections | (Δ/σ)max = 0.001 |
326 parameters | Δρmax = 0.84 e Å−3 |
0 restraints | Δρmin = −0.61 e Å−3 |
[Pd(C15H11N3)(C2H3N)](PF6)2 | V = 2254.42 (10) Å3 |
Mr = 670.66 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.1073 (3) Å | µ = 1.08 mm−1 |
b = 11.8840 (3) Å | T = 273 K |
c = 14.6085 (4) Å | 0.30 × 0.24 × 0.22 mm |
β = 97.810 (1)° |
Bruker SMART diffractometer | 5449 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 4503 reflections with I > 2σ(I) |
Tmin = 0.738, Tmax = 0.797 | Rint = 0.017 |
16715 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | 0 restraints |
wR(F2) = 0.142 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.84 e Å−3 |
5449 reflections | Δρmin = −0.61 e Å−3 |
326 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 | ||
Pd1 | 0.76117 (2) | 0.28974 (2) | 0.599820 (18) | 0.04089 (12) | |
N1 | 0.6996 (2) | 0.3828 (3) | 0.6946 (2) | 0.0479 (7) | |
N2 | 0.7149 (2) | 0.1693 (3) | 0.6726 (2) | 0.0426 (6) | |
N3 | 0.8072 (2) | 0.1568 (3) | 0.5289 (2) | 0.0444 (6) | |
N4 | 0.8108 (3) | 0.4156 (3) | 0.5235 (2) | 0.0527 (8) | |
C1 | 0.6934 (3) | 0.4957 (4) | 0.6996 (3) | 0.0570 (10) | |
H1 | 0.7211 | 0.5393 | 0.6562 | 0.068* | |
C2 | 0.6472 (4) | 0.5483 (5) | 0.7672 (4) | 0.0691 (12) | |
H2 | 0.6433 | 0.6263 | 0.7692 | 0.083* | |
C3 | 0.6070 (4) | 0.4841 (5) | 0.8313 (3) | 0.0695 (13) | |
H3 | 0.5765 | 0.5187 | 0.8779 | 0.083* | |
C4 | 0.6115 (3) | 0.3684 (5) | 0.8272 (3) | 0.0617 (11) | |
H4 | 0.5833 | 0.3241 | 0.8699 | 0.074* | |
C5 | 0.6589 (3) | 0.3196 (4) | 0.7584 (3) | 0.0498 (8) | |
C6 | 0.6679 (3) | 0.1969 (4) | 0.7459 (3) | 0.0489 (9) | |
C7 | 0.6330 (4) | 0.1121 (4) | 0.7987 (3) | 0.0622 (11) | |
H7 | 0.5998 | 0.1286 | 0.8494 | 0.075* | |
C8 | 0.6495 (4) | 0.0009 (4) | 0.7734 (3) | 0.0691 (13) | |
H8 | 0.6265 | −0.0574 | 0.8079 | 0.083* | |
C9 | 0.6985 (4) | −0.0243 (4) | 0.6990 (3) | 0.0615 (11) | |
H9 | 0.7095 | −0.0988 | 0.6832 | 0.074* | |
C10 | 0.7317 (3) | 0.0635 (3) | 0.6473 (3) | 0.0475 (8) | |
C11 | 0.7857 (3) | 0.0558 (3) | 0.5664 (3) | 0.0468 (8) | |
C12 | 0.8143 (4) | −0.0446 (4) | 0.5296 (3) | 0.0594 (10) | |
H12 | 0.8001 | −0.1127 | 0.5567 | 0.071* | |
C13 | 0.8644 (4) | −0.0430 (4) | 0.4523 (4) | 0.0664 (12) | |
H13 | 0.8837 | −0.1098 | 0.4263 | 0.080* | |
C14 | 0.8852 (4) | 0.0591 (4) | 0.4143 (3) | 0.0648 (11) | |
H14 | 0.9185 | 0.0619 | 0.3621 | 0.078* | |
C15 | 0.8562 (3) | 0.1575 (4) | 0.4544 (3) | 0.0533 (9) | |
H15 | 0.8713 | 0.2261 | 0.4287 | 0.064* | |
C16 | 0.8393 (3) | 0.4869 (4) | 0.4829 (3) | 0.0554 (9) | |
C17 | 0.8762 (4) | 0.5793 (4) | 0.4315 (4) | 0.0729 (13) | |
H17A | 0.8209 | 0.6312 | 0.4137 | 0.109* | |
H17B | 0.9011 | 0.5506 | 0.3772 | 0.109* | |
H17C | 0.9310 | 0.6174 | 0.4695 | 0.109* | |
P1 | 0.42931 (10) | 0.28021 (9) | 0.51579 (8) | 0.0546 (3) | |
F1 | 0.3845 (4) | 0.4019 (3) | 0.5203 (3) | 0.1248 (16) | |
F2 | 0.4705 (4) | 0.2847 (4) | 0.6212 (3) | 0.1263 (17) | |
F3 | 0.4664 (6) | 0.1569 (4) | 0.5074 (4) | 0.177 (3) | |
F4 | 0.3944 (6) | 0.2746 (5) | 0.4096 (3) | 0.158 (3) | |
F5 | 0.5332 (4) | 0.3245 (6) | 0.4898 (4) | 0.158 (2) | |
F6 | 0.3290 (4) | 0.2329 (6) | 0.5489 (5) | 0.160 (2) | |
P2 | 0.02951 (11) | 0.19057 (12) | 0.77715 (10) | 0.0668 (3) | |
F7 | 0.1387 (4) | 0.2137 (5) | 0.7471 (4) | 0.142 (2) | |
F8 | 0.0705 (5) | 0.0699 (4) | 0.8046 (5) | 0.169 (2) | |
F9 | −0.0789 (4) | 0.1664 (6) | 0.8057 (4) | 0.162 (2) | |
F10 | −0.0074 (9) | 0.3078 (6) | 0.7566 (6) | 0.237 (5) | |
F11 | 0.0641 (5) | 0.2300 (6) | 0.8785 (4) | 0.156 (2) | |
F12 | −0.0095 (4) | 0.1471 (8) | 0.6798 (4) | 0.222 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.04320 (18) | 0.04512 (18) | 0.03571 (17) | −0.00289 (10) | 0.01025 (11) | 0.00267 (10) |
N1 | 0.0457 (16) | 0.0548 (18) | 0.0442 (16) | 0.0007 (13) | 0.0104 (13) | −0.0044 (14) |
N2 | 0.0403 (15) | 0.0500 (16) | 0.0381 (15) | −0.0042 (12) | 0.0075 (11) | 0.0078 (12) |
N3 | 0.0465 (16) | 0.0477 (16) | 0.0404 (15) | −0.0032 (13) | 0.0104 (12) | 0.0006 (12) |
N4 | 0.060 (2) | 0.0489 (18) | 0.0509 (18) | −0.0043 (15) | 0.0158 (15) | 0.0032 (14) |
C1 | 0.059 (2) | 0.055 (2) | 0.059 (2) | 0.0008 (18) | 0.0123 (19) | −0.0036 (19) |
C2 | 0.074 (3) | 0.066 (3) | 0.068 (3) | 0.007 (2) | 0.014 (2) | −0.016 (2) |
C3 | 0.062 (3) | 0.087 (3) | 0.062 (3) | 0.003 (2) | 0.017 (2) | −0.025 (2) |
C4 | 0.052 (2) | 0.089 (3) | 0.046 (2) | −0.004 (2) | 0.0154 (17) | −0.007 (2) |
C5 | 0.045 (2) | 0.064 (2) | 0.0416 (19) | −0.0035 (17) | 0.0073 (15) | −0.0025 (17) |
C6 | 0.045 (2) | 0.065 (2) | 0.0379 (18) | −0.0058 (16) | 0.0086 (15) | 0.0039 (16) |
C7 | 0.062 (3) | 0.082 (3) | 0.046 (2) | −0.011 (2) | 0.0207 (18) | 0.011 (2) |
C8 | 0.080 (3) | 0.071 (3) | 0.059 (3) | −0.016 (2) | 0.018 (2) | 0.019 (2) |
C9 | 0.073 (3) | 0.054 (2) | 0.059 (2) | −0.012 (2) | 0.014 (2) | 0.0103 (19) |
C10 | 0.051 (2) | 0.050 (2) | 0.0421 (18) | −0.0074 (16) | 0.0079 (15) | 0.0032 (15) |
C11 | 0.049 (2) | 0.0482 (19) | 0.0426 (18) | −0.0057 (15) | 0.0057 (15) | 0.0004 (15) |
C12 | 0.066 (3) | 0.049 (2) | 0.063 (3) | −0.0027 (19) | 0.009 (2) | −0.0033 (19) |
C13 | 0.070 (3) | 0.061 (3) | 0.071 (3) | 0.004 (2) | 0.021 (2) | −0.014 (2) |
C14 | 0.066 (3) | 0.077 (3) | 0.056 (2) | −0.001 (2) | 0.025 (2) | −0.009 (2) |
C15 | 0.053 (2) | 0.061 (2) | 0.049 (2) | −0.0060 (18) | 0.0181 (17) | −0.0010 (18) |
C16 | 0.063 (2) | 0.051 (2) | 0.055 (2) | −0.0025 (18) | 0.0167 (18) | 0.0043 (18) |
C17 | 0.083 (3) | 0.065 (3) | 0.074 (3) | −0.013 (2) | 0.022 (2) | 0.016 (2) |
P1 | 0.0650 (7) | 0.0540 (6) | 0.0473 (6) | −0.0014 (5) | 0.0168 (5) | −0.0016 (4) |
F1 | 0.197 (5) | 0.083 (2) | 0.103 (3) | 0.043 (3) | 0.051 (3) | 0.006 (2) |
F2 | 0.132 (4) | 0.175 (5) | 0.067 (2) | 0.031 (3) | −0.001 (2) | −0.009 (2) |
F3 | 0.344 (9) | 0.075 (3) | 0.137 (4) | 0.073 (4) | 0.126 (5) | 0.025 (3) |
F4 | 0.256 (7) | 0.143 (5) | 0.063 (2) | 0.043 (4) | −0.019 (3) | −0.013 (2) |
F5 | 0.137 (4) | 0.197 (5) | 0.158 (5) | −0.049 (4) | 0.092 (4) | −0.011 (4) |
F6 | 0.095 (3) | 0.179 (5) | 0.214 (6) | −0.044 (3) | 0.054 (4) | 0.012 (5) |
P2 | 0.0668 (8) | 0.0756 (8) | 0.0582 (7) | 0.0143 (6) | 0.0093 (6) | −0.0119 (6) |
F7 | 0.114 (4) | 0.171 (6) | 0.150 (5) | −0.014 (3) | 0.050 (3) | −0.007 (3) |
F8 | 0.164 (5) | 0.096 (3) | 0.247 (7) | 0.030 (3) | 0.030 (4) | 0.008 (4) |
F9 | 0.095 (3) | 0.249 (6) | 0.153 (4) | −0.027 (4) | 0.058 (3) | −0.093 (5) |
F10 | 0.367 (12) | 0.145 (5) | 0.225 (8) | 0.141 (7) | 0.138 (8) | 0.061 (5) |
F11 | 0.146 (4) | 0.230 (6) | 0.087 (3) | −0.021 (4) | −0.004 (3) | −0.046 (4) |
F12 | 0.126 (4) | 0.430 (12) | 0.100 (3) | 0.089 (6) | −0.015 (3) | −0.124 (6) |
Pd1—N1 | 2.023 (3) | C9—H9 | 0.9300 |
Pd1—N2 | 1.929 (3) | C10—C11 | 1.461 (6) |
Pd1—N3 | 2.026 (3) | C11—C12 | 1.381 (6) |
Pd1—N4 | 2.025 (3) | C12—C13 | 1.381 (7) |
N1—C1 | 1.346 (5) | C12—H12 | 0.9300 |
N1—C5 | 1.362 (5) | C13—C14 | 1.377 (7) |
N2—C10 | 1.338 (5) | C13—H13 | 0.9300 |
N2—C6 | 1.346 (5) | C14—C15 | 1.383 (6) |
N3—C15 | 1.337 (5) | C14—H14 | 0.9300 |
N3—C11 | 1.365 (5) | C15—H15 | 0.9300 |
N4—C16 | 1.126 (5) | C16—C17 | 1.451 (6) |
C1—C2 | 1.377 (6) | C17—H17A | 0.9600 |
C1—H1 | 0.9300 | C17—H17B | 0.9600 |
C2—C3 | 1.367 (8) | C17—H17C | 0.9600 |
C2—H2 | 0.9300 | P1—F3 | 1.554 (4) |
C3—C4 | 1.379 (7) | P1—F5 | 1.555 (4) |
C3—H3 | 0.9300 | P1—F4 | 1.558 (5) |
C4—C5 | 1.379 (6) | P1—F2 | 1.561 (4) |
C4—H4 | 0.9300 | P1—F6 | 1.566 (5) |
C5—C6 | 1.477 (6) | P1—F1 | 1.566 (4) |
C6—C7 | 1.384 (6) | P2—F10 | 1.491 (6) |
C7—C8 | 1.397 (7) | P2—F12 | 1.533 (5) |
C7—H7 | 0.9300 | P2—F9 | 1.561 (5) |
C8—C9 | 1.369 (7) | P2—F11 | 1.561 (5) |
C8—H8 | 0.9300 | P2—F8 | 1.565 (5) |
C9—C10 | 1.391 (5) | P2—F7 | 1.578 (5) |
N2—Pd1—N1 | 81.0 (1) | C11—C12—C13 | 119.4 (4) |
N2—Pd1—N4 | 179.6 (1) | C11—C12—H12 | 120.3 |
N1—Pd1—N4 | 99.2 (1) | C13—C12—H12 | 120.3 |
N2—Pd1—N3 | 80.9 (1) | C14—C13—C12 | 118.9 (4) |
N1—Pd1—N3 | 161.9 (1) | C14—C13—H13 | 120.5 |
N4—Pd1—N3 | 98.9 (1) | C12—C13—H13 | 120.5 |
C1—N1—C5 | 118.7 (4) | C13—C14—C15 | 119.6 (4) |
C1—N1—Pd1 | 127.9 (3) | C13—C14—H14 | 120.2 |
C5—N1—Pd1 | 113.4 (3) | C15—C14—H14 | 120.2 |
C10—N2—C6 | 123.9 (3) | N3—C15—C14 | 122.0 (4) |
C10—N2—Pd1 | 118.0 (2) | N3—C15—H15 | 119.0 |
C6—N2—Pd1 | 118.0 (3) | C14—C15—H15 | 119.0 |
C15—N3—C11 | 118.7 (3) | N4—C16—C17 | 179.5 (5) |
C15—N3—Pd1 | 128.4 (3) | C16—C17—H17A | 109.5 |
C11—N3—Pd1 | 112.9 (2) | C16—C17—H17B | 109.5 |
C16—N4—Pd1 | 178.3 (4) | H17A—C17—H17B | 109.5 |
N1—C1—C2 | 121.8 (4) | C16—C17—H17C | 109.5 |
N1—C1—H1 | 119.1 | H17A—C17—H17C | 109.5 |
C2—C1—H1 | 119.1 | H17B—C17—H17C | 109.5 |
C3—C2—C1 | 119.1 (5) | F3—P1—F5 | 90.3 (4) |
C3—C2—H2 | 120.4 | F3—P1—F4 | 86.2 (3) |
C1—C2—H2 | 120.4 | F5—P1—F4 | 85.4 (4) |
C2—C3—C4 | 120.2 (4) | F3—P1—F2 | 92.3 (3) |
C2—C3—H3 | 119.9 | F5—P1—F2 | 91.8 (3) |
C4—C3—H3 | 119.9 | F4—P1—F2 | 176.8 (4) |
C3—C4—C5 | 118.5 (5) | F3—P1—F6 | 88.3 (4) |
C3—C4—H4 | 120.7 | F5—P1—F6 | 175.8 (4) |
C5—C4—H4 | 120.7 | F4—P1—F6 | 98.5 (4) |
N1—C5—C4 | 121.6 (4) | F2—P1—F6 | 84.3 (3) |
N1—C5—C6 | 114.5 (3) | F3—P1—F1 | 176.0 (4) |
C4—C5—C6 | 123.8 (4) | F5—P1—F1 | 92.5 (3) |
N2—C6—C7 | 119.2 (4) | F4—P1—F1 | 91.2 (3) |
N2—C6—C5 | 113.1 (3) | F2—P1—F1 | 90.5 (3) |
C7—C6—C5 | 127.7 (4) | F6—P1—F1 | 89.0 (3) |
C6—C7—C8 | 117.8 (4) | F10—P2—F12 | 94.0 (5) |
C6—C7—H7 | 121.1 | F10—P2—F9 | 86.8 (5) |
C8—C7—H7 | 121.1 | F12—P2—F9 | 89.1 (3) |
C9—C8—C7 | 121.5 (4) | F10—P2—F11 | 87.4 (5) |
C9—C8—H8 | 119.2 | F12—P2—F11 | 176.4 (5) |
C7—C8—H8 | 119.2 | F9—P2—F11 | 87.7 (3) |
C8—C9—C10 | 118.8 (4) | F10—P2—F8 | 176.7 (5) |
C8—C9—H9 | 120.6 | F12—P2—F8 | 89.3 (4) |
C10—C9—H9 | 120.6 | F9—P2—F8 | 93.2 (4) |
N2—C10—C9 | 118.7 (4) | F11—P2—F8 | 89.2 (4) |
N2—C10—C11 | 113.5 (3) | F10—P2—F7 | 93.6 (5) |
C9—C10—C11 | 127.8 (4) | F12—P2—F7 | 90.1 (4) |
N3—C11—C12 | 121.5 (4) | F9—P2—F7 | 179.1 (3) |
N3—C11—C10 | 114.8 (3) | F11—P2—F7 | 93.1 (3) |
C12—C11—C10 | 123.8 (4) | F8—P2—F7 | 86.4 (3) |
N2—Pd1—N1—C1 | −178.6 (4) | Pd1—N2—C6—C5 | 0.3 (4) |
N4—Pd1—N1—C1 | 1.7 (4) | N1—C5—C6—N2 | −0.3 (5) |
N3—Pd1—N1—C1 | −178.3 (4) | C4—C5—C6—N2 | 178.4 (4) |
N2—Pd1—N1—C5 | 0.0 (3) | N1—C5—C6—C7 | −179.3 (4) |
N4—Pd1—N1—C5 | −179.7 (3) | C4—C5—C6—C7 | −0.6 (7) |
N3—Pd1—N1—C5 | 0.3 (6) | N2—C6—C7—C8 | 0.5 (7) |
N1—Pd1—N2—C10 | 179.9 (3) | C5—C6—C7—C8 | 179.5 (4) |
N3—Pd1—N2—C10 | 0.0 (3) | C6—C7—C8—C9 | 0.1 (8) |
N1—Pd1—N2—C6 | −0.1 (3) | C7—C8—C9—C10 | −0.6 (8) |
N3—Pd1—N2—C6 | 180.0 (3) | C6—N2—C10—C9 | 0.2 (6) |
N2—Pd1—N3—C15 | −179.3 (4) | Pd1—N2—C10—C9 | −179.8 (3) |
N1—Pd1—N3—C15 | −179.7 (4) | C6—N2—C10—C11 | −179.1 (3) |
N4—Pd1—N3—C15 | 0.3 (4) | Pd1—N2—C10—C11 | 0.9 (5) |
N2—Pd1—N3—C11 | −1.0 (3) | C8—C9—C10—N2 | 0.4 (7) |
N1—Pd1—N3—C11 | −1.3 (6) | C8—C9—C10—C11 | 179.6 (4) |
N4—Pd1—N3—C11 | 178.7 (3) | C15—N3—C11—C12 | 0.8 (6) |
C5—N1—C1—C2 | 0.0 (7) | Pd1—N3—C11—C12 | −177.7 (3) |
Pd1—N1—C1—C2 | 178.6 (3) | C15—N3—C11—C10 | −179.8 (4) |
N1—C1—C2—C3 | 0.4 (8) | Pd1—N3—C11—C10 | 1.7 (4) |
C1—C2—C3—C4 | −1.0 (8) | N2—C10—C11—N3 | −1.7 (5) |
C2—C3—C4—C5 | 1.2 (8) | C9—C10—C11—N3 | 179.1 (4) |
C1—N1—C5—C4 | 0.2 (6) | N2—C10—C11—C12 | 177.7 (4) |
Pd1—N1—C5—C4 | −178.6 (3) | C9—C10—C11—C12 | −1.5 (7) |
C1—N1—C5—C6 | 178.9 (4) | N3—C11—C12—C13 | −1.2 (7) |
Pd1—N1—C5—C6 | 0.2 (4) | C10—C11—C12—C13 | 179.4 (4) |
C3—C4—C5—N1 | −0.8 (7) | C11—C12—C13—C14 | 0.6 (8) |
C3—C4—C5—C6 | −179.4 (4) | C12—C13—C14—C15 | 0.3 (8) |
C10—N2—C6—C7 | −0.7 (6) | C11—N3—C15—C14 | 0.2 (6) |
Pd1—N2—C6—C7 | 179.4 (3) | Pd1—N3—C15—C14 | 178.4 (3) |
C10—N2—C6—C5 | −179.8 (3) | C13—C14—C15—N3 | −0.7 (7) |
D—H···A | D—H | H···A | D···A | D—H···A |
C15—H15···F9i | 0.93 | 2.37 | 3.213 (6) | 151 |
C14—H14···F10i | 0.93 | 2.47 | 3.268 (9) | 143 |
C13—H13···F12ii | 0.93 | 2.45 | 3.142 (7) | 131 |
C7—H7···F5iii | 0.93 | 2.40 | 3.326 (7) | 173 |
C3—H3···F3iv | 0.93 | 2.47 | 3.363 (7) | 162 |
P1—F2···Cg1 | ? | 2.95 | 3.062 (5) | 122 (1) |
P2—F12···Cg2v | ? | 2.97 | 3.075 (6) | 122 (1) |
Symmetry codes: (i) x+1, −y+1/2, z−1/2; (ii) −x+1, −y, −z+1; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+3/2; (v) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Pd(C15H11N3)(C2H3N)](PF6)2 |
Mr | 670.66 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 273 |
a, b, c (Å) | 13.1073 (3), 11.8840 (3), 14.6085 (4) |
β (°) | 97.810 (1) |
V (Å3) | 2254.42 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.08 |
Crystal size (mm) | 0.30 × 0.24 × 0.22 |
Data collection | |
Diffractometer | Bruker SMART |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.738, 0.797 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 16715, 5449, 4503 |
Rint | 0.017 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.142, 1.06 |
No. of reflections | 5449 |
No. of parameters | 326 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.84, −0.61 |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXTL (Sheldrick, 2001), SHELXTL.
Pd1—N1 | 2.023 (3) | Pd1—N3 | 2.026 (3) |
Pd1—N2 | 1.929 (3) | Pd1—N4 | 2.025 (3) |
N2—Pd1—N1 | 81.0 (1) | N2—Pd1—N3 | 80.9 (1) |
N2—Pd1—N4 | 179.6 (1) | N1—Pd1—N3 | 161.9 (1) |
D—H···A | D—H | H···A | D···A | D—H···A |
C15—H15···F9i | 0.93 | 2.37 | 3.213 (6) | 151 |
C14—H14···F10i | 0.93 | 2.47 | 3.268 (9) | 143 |
C13—H13···F12ii | 0.93 | 2.45 | 3.142 (7) | 131 |
C7—H7···F5iii | 0.93 | 2.40 | 3.326 (7) | 173 |
C3—H3···F3iv | 0.93 | 2.47 | 3.363 (7) | 162 |
P1—F2···Cg1 | ? | 2.95 | 3.062 (5) | 122.3 (3) |
P2—F12···Cg2v | ? | 2.97 | 3.075 (6) | 121.7 (3) |
Symmetry codes: (i) x+1, −y+1/2, z−1/2; (ii) −x+1, −y, −z+1; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+3/2; (v) x−1, y, z. |
The 2,2':6',2''-terpyridine complexes of palladium(II) and platinum(II) have the metal centers in a square-planar geometry (Angle et al., 2006; Onoda et al., 2003; Roszak et al., 1996). The title compound also displays square-planar coordination, with four N atoms from terpy and acetonitrile molecule (Fig. 1). The crystal structure comprises alternating layers of cations and anions as represented in Fig. 2. The compound packs by an anion–π interaction (P1—F2···Cg1 3.063 (5) Å [Cg1 is the centroid of the ring system Pd1, N1, C5, C6, N2; P2—F12···Cg2 3.076 (6) Å, Cg2 is the centroid of the ring system Pd1, N2, C10, C11, N3] and hydrogen bonds involving hexafluorophosphate anions (C—H···F). Non-classical hydrogen bonds that connect cations, anions and coordinated acetonitrile molecules are detailed in Table 2.