Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010902839X/gz3165sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827010902839X/gz3165Isup2.hkl |
CCDC reference: 746051
Pt(2,2'-bipyridine)Cl2 (20 mg) was treated with Ag(O2CCF3) (42 mg) (\sim 1:4 ratio) in the presence of KCl (3.6 mg, ~1 equivalent) in CH2Cl2 (20 ml). The reaction mixture was stirred for 2 h at room temperature in the dark. After filtration, the yellow solution was evaporated slowly to give yellow crystals of (I) as a minor product.
The disorder associated with atoms F7, F8 and F9 was modelled as two orientations with occupancies which summed to unity, of 0.617 (7) and 0.383 (7) for parts A and B, respectively. Atoms F13, F14 and F15 were modelled similarly, with occupancies of 0.542 (7) and 0.458 (7) for parts A and B, respectively. Atoms F10, F11 and F12 were modelled as three orientations with occupancies which summed to unity, of 0.460 (9), 0.306 (7) and 0.234 (9) for F10/F11/F12 parts A, B and C, respectively. The C—F bond lengths for atom F10–F15 were restrained to 1.330 (5) Å to stabilize the refinement, and F atoms from all three disordered –CF3 groups were each constrained to common displacement parameters. F···F distances in these cases were further modelled using distance restraints [SADI, FLAT (SHELXL97; Sheldrick, 2008)] as necessary. All H atoms were assigned to geometrically idealized positions with C—H bond lengths of 0.93 Å, and were constrained to ride on their parent C atoms with Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 2007); cell refinement: SMART (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) and Mercury (Macrae et al., 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
K2[Pt2Ag8(C10H8N2)2(C2F3O2)14] | Z = 1 |
Mr = 3225.98 | F(000) = 1504 |
Triclinic, P1 | Dx = 2.705 Mg m−3 |
a = 11.9829 (6) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.4737 (6) Å | Cell parameters from 9980 reflections |
c = 14.4368 (7) Å | θ = 2.4–27.9° |
α = 77.378 (1)° | µ = 5.73 mm−1 |
β = 70.132 (1)° | T = 296 K |
γ = 86.305 (1)° | Block, yellow |
V = 1980.28 (17) Å3 | 0.10 × 0.10 × 0.05 mm |
Bruker SMART CCD area-detector diffractometer | 7748 independent reflections |
Radiation source: sealed tube | 7189 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
ϕ and ω scans | θmax = 26.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Bruker, 2008) | h = −14→14 |
Tmin = 0.598, Tmax = 0.763 | k = −15→15 |
20732 measured reflections | l = −17→17 |
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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.058 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0247P)2 + 5.4864P] where P = (Fo2 + 2Fc2)/3 |
7748 reflections | (Δ/σ)max = 0.011 |
609 parameters | Δρmax = 0.97 e Å−3 |
112 restraints | Δρmin = −1.24 e Å−3 |
K2[Pt2Ag8(C10H8N2)2(C2F3O2)14] | γ = 86.305 (1)° |
Mr = 3225.98 | V = 1980.28 (17) Å3 |
Triclinic, P1 | Z = 1 |
a = 11.9829 (6) Å | Mo Kα radiation |
b = 12.4737 (6) Å | µ = 5.73 mm−1 |
c = 14.4368 (7) Å | T = 296 K |
α = 77.378 (1)° | 0.10 × 0.10 × 0.05 mm |
β = 70.132 (1)° |
Bruker SMART CCD area-detector diffractometer | 7748 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2008) | 7189 reflections with I > 2σ(I) |
Tmin = 0.598, Tmax = 0.763 | Rint = 0.018 |
20732 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 112 restraints |
wR(F2) = 0.058 | H-atom parameters constrained |
S = 1.03 | Δρmax = 0.97 e Å−3 |
7748 reflections | Δρmin = −1.24 e Å−3 |
609 parameters |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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) | |
Pt1 | 0.508344 (14) | 0.462548 (13) | 0.120846 (12) | 0.02291 (5) | |
K1 | 0.71700 (8) | 0.09964 (8) | 0.32322 (7) | 0.0294 (2) | |
Ag1 | 0.50746 (3) | 0.33688 (3) | 0.31804 (3) | 0.03095 (8) | |
Ag2 | 0.45421 (3) | 0.16602 (3) | 0.53951 (3) | 0.03641 (9) | |
Ag3 | 0.40367 (3) | 0.38620 (3) | 0.59063 (3) | 0.03883 (9) | |
Ag4 | 0.11801 (3) | −0.04212 (3) | 0.48116 (3) | 0.03432 (9) | |
C1 | 0.4210 (5) | 0.6544 (4) | 0.2127 (4) | 0.0364 (11) | |
H1A | 0.5005 | 0.6706 | 0.1989 | 0.044* | |
C2 | 0.3344 (5) | 0.7209 (4) | 0.2613 (4) | 0.0453 (13) | |
H2A | 0.3555 | 0.7805 | 0.2812 | 0.054* | |
C3 | 0.2178 (5) | 0.6991 (4) | 0.2800 (4) | 0.0420 (12) | |
H3A | 0.1590 | 0.7443 | 0.3115 | 0.050* | |
C4 | 0.1881 (4) | 0.6096 (4) | 0.2517 (4) | 0.0358 (11) | |
H4A | 0.1089 | 0.5935 | 0.2643 | 0.043* | |
C5 | 0.2765 (4) | 0.5437 (4) | 0.2044 (3) | 0.0274 (9) | |
C6 | 0.2584 (4) | 0.4466 (4) | 0.1694 (3) | 0.0276 (9) | |
C7 | 0.1491 (4) | 0.4064 (4) | 0.1790 (4) | 0.0372 (11) | |
H7A | 0.0797 | 0.4415 | 0.2095 | 0.045* | |
C8 | 0.1442 (5) | 0.3148 (5) | 0.1431 (4) | 0.0447 (13) | |
H8A | 0.0713 | 0.2864 | 0.1498 | 0.054* | |
C9 | 0.2478 (5) | 0.2646 (4) | 0.0970 (4) | 0.0406 (12) | |
H9A | 0.2455 | 0.2025 | 0.0718 | 0.049* | |
C10 | 0.3550 (4) | 0.3075 (4) | 0.0887 (3) | 0.0306 (10) | |
H10A | 0.4251 | 0.2740 | 0.0571 | 0.037* | |
C11 | 0.7974 (5) | 0.2539 (5) | 0.0205 (4) | 0.0486 (14) | |
C12 | 0.6888 (4) | 0.2978 (4) | 0.0955 (3) | 0.0297 (10) | |
C13 | 0.3730 (5) | 0.0708 (4) | 0.2911 (4) | 0.0378 (11) | |
C14 | 0.3921 (4) | 0.0600 (4) | 0.3928 (3) | 0.0280 (9) | |
C15 | 0.1169 (4) | 0.3183 (3) | 0.4796 (3) | 0.0383 (11) | |
C16 | 0.2513 (4) | 0.3222 (4) | 0.4586 (4) | 0.0310 (10) | |
C17 | −0.0114 (4) | 0.0384 (3) | 0.7861 (4) | 0.0491 (14) | |
C18 | −0.0074 (4) | 0.0223 (4) | 0.6826 (4) | 0.0334 (10) | |
C19 | 0.3244 (4) | 0.0900 (4) | 0.8708 (4) | 0.0554 (16) | |
C20 | 0.3595 (4) | 0.1486 (4) | 0.7593 (4) | 0.0357 (11) | |
C21 | 0.8005 (4) | 0.3563 (4) | 0.4246 (4) | 0.0353 (11) | |
C22 | 0.6650 (4) | 0.3463 (4) | 0.4570 (3) | 0.0269 (9) | |
C23 | 0.8241 (4) | 0.5726 (5) | 0.1532 (4) | 0.0409 (12) | |
C24 | 0.6953 (4) | 0.5311 (4) | 0.1865 (4) | 0.0302 (10) | |
N1 | 0.3926 (3) | 0.5676 (3) | 0.1853 (3) | 0.0259 (8) | |
N2 | 0.3602 (3) | 0.3960 (3) | 0.1250 (3) | 0.0249 (7) | |
O1 | 0.6232 (3) | 0.3549 (3) | 0.0505 (2) | 0.0309 (7) | |
O2 | 0.6786 (3) | 0.2775 (3) | 0.1848 (2) | 0.0324 (7) | |
O3 | 0.4766 (3) | 0.1142 (3) | 0.3910 (2) | 0.0333 (7) | |
O4 | 0.3205 (3) | −0.0008 (3) | 0.4652 (3) | 0.0444 (9) | |
O5 | 0.3101 (3) | 0.3469 (3) | 0.3685 (3) | 0.0499 (10) | |
O6 | 0.2820 (3) | 0.2963 (3) | 0.5336 (3) | 0.0454 (9) | |
O7 | 0.0758 (3) | −0.0349 (3) | 0.6416 (3) | 0.0401 (8) | |
O8 | −0.0877 (3) | 0.0675 (3) | 0.6532 (2) | 0.0359 (8) | |
O9 | 0.3728 (4) | 0.0859 (3) | 0.7002 (3) | 0.0454 (9) | |
O10 | 0.3731 (3) | 0.2486 (3) | 0.7426 (3) | 0.0429 (9) | |
O11 | 0.6306 (3) | 0.2661 (3) | 0.4343 (2) | 0.0318 (7) | |
O12 | 0.6067 (3) | 0.4149 (3) | 0.5036 (2) | 0.0332 (7) | |
O13 | 0.6597 (3) | 0.5364 (3) | 0.1117 (2) | 0.0308 (7) | |
O14 | 0.6440 (3) | 0.4944 (3) | 0.2755 (2) | 0.0334 (7) | |
F1 | 0.8703 (3) | 0.3362 (3) | −0.0368 (3) | 0.0692 (11) | |
F2 | 0.8565 (4) | 0.1821 (4) | 0.0679 (3) | 0.0849 (14) | |
F3 | 0.7661 (3) | 0.2044 (3) | −0.0397 (2) | 0.0631 (10) | |
F4 | 0.4565 (3) | 0.1324 (3) | 0.2148 (2) | 0.0546 (8) | |
F5 | 0.2691 (3) | 0.1174 (3) | 0.2945 (3) | 0.0567 (9) | |
F6 | 0.3717 (4) | −0.0255 (3) | 0.2677 (3) | 0.0633 (10) | |
F7B | 0.0821 (9) | 0.2171 (5) | 0.4859 (8) | 0.0581 (10) | 0.383 (7) |
F8B | 0.0545 (8) | 0.3464 (8) | 0.5667 (5) | 0.0581 (10) | 0.383 (7) |
F9B | 0.0806 (9) | 0.3859 (7) | 0.4107 (6) | 0.0581 (10) | 0.383 (7) |
F7A | 0.0902 (5) | 0.2382 (4) | 0.4422 (5) | 0.0581 (10) | 0.62 |
F8A | 0.0522 (5) | 0.2993 (5) | 0.5765 (3) | 0.0581 (10) | 0.62 |
F9A | 0.0800 (6) | 0.4128 (4) | 0.4365 (5) | 0.0581 (10) | 0.62 |
F10A | 0.0838 (8) | 0.0011 (10) | 0.8108 (7) | 0.0623 (13) | 0.460 (9) |
F11A | −0.0153 (11) | 0.1460 (4) | 0.7871 (6) | 0.0623 (13) | 0.460 (9) |
F12A | −0.1102 (7) | −0.0031 (9) | 0.8583 (5) | 0.0623 (13) | 0.460 (9) |
F10B | 0.1004 (6) | 0.0386 (11) | 0.7888 (9) | 0.0623 (13) | 0.306 (8) |
F11B | −0.0558 (12) | 0.1303 (8) | 0.8137 (9) | 0.0623 (13) | 0.306 (8) |
F12B | −0.0592 (12) | −0.0494 (7) | 0.8577 (6) | 0.0623 (13) | 0.306 (8) |
F10C | 0.0326 (18) | −0.0455 (11) | 0.8353 (10) | 0.0623 (13) | 0.234 (9) |
F11C | 0.0293 (15) | 0.1363 (8) | 0.7805 (10) | 0.0623 (13) | 0.234 (9) |
F12C | −0.1270 (6) | 0.0424 (17) | 0.8429 (10) | 0.0623 (13) | 0.234 (9) |
F13B | 0.3643 (8) | −0.0125 (5) | 0.8879 (6) | 0.0692 (12) | 0.458 (7) |
F14B | 0.3815 (8) | 0.1445 (6) | 0.9136 (7) | 0.0692 (12) | 0.458 (7) |
F15B | 0.2127 (6) | 0.0941 (7) | 0.9279 (7) | 0.0692 (12) | 0.458 (7) |
F13A | 0.3060 (8) | −0.0178 (4) | 0.8807 (5) | 0.0692 (12) | 0.54 |
F14A | 0.3965 (7) | 0.1056 (6) | 0.9176 (6) | 0.0692 (12) | 0.54 |
F15A | 0.2151 (5) | 0.1245 (6) | 0.9160 (6) | 0.0692 (12) | 0.54 |
F16 | 0.8556 (3) | 0.3324 (3) | 0.3356 (3) | 0.0653 (10) | |
F17 | 0.8387 (3) | 0.2843 (3) | 0.4909 (3) | 0.0541 (8) | |
F18 | 0.8387 (3) | 0.4544 (3) | 0.4208 (3) | 0.0624 (10) | |
F19 | 0.8969 (3) | 0.4935 (3) | 0.1213 (3) | 0.0719 (11) | |
F20 | 0.8508 (3) | 0.5955 (3) | 0.2279 (3) | 0.0626 (10) | |
F21 | 0.8486 (3) | 0.6605 (3) | 0.0799 (3) | 0.0635 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.02069 (8) | 0.02421 (9) | 0.02130 (8) | 0.00181 (6) | −0.00703 (6) | −0.00005 (6) |
K1 | 0.0294 (5) | 0.0276 (5) | 0.0322 (5) | 0.0048 (4) | −0.0126 (4) | −0.0058 (4) |
Ag1 | 0.02294 (16) | 0.03481 (19) | 0.02878 (17) | −0.00196 (13) | −0.00763 (13) | 0.00529 (14) |
Ag2 | 0.0409 (2) | 0.0391 (2) | 0.02886 (18) | −0.00081 (16) | −0.00902 (15) | −0.01014 (15) |
Ag3 | 0.0392 (2) | 0.0329 (2) | 0.0426 (2) | −0.00174 (16) | −0.01206 (17) | −0.00598 (16) |
Ag4 | 0.02935 (18) | 0.0429 (2) | 0.03540 (19) | 0.00666 (15) | −0.01387 (15) | −0.01473 (16) |
C1 | 0.038 (3) | 0.026 (2) | 0.047 (3) | 0.000 (2) | −0.018 (2) | −0.005 (2) |
C2 | 0.055 (3) | 0.031 (3) | 0.054 (3) | 0.007 (2) | −0.020 (3) | −0.017 (2) |
C3 | 0.050 (3) | 0.035 (3) | 0.041 (3) | 0.019 (2) | −0.014 (2) | −0.014 (2) |
C4 | 0.029 (2) | 0.040 (3) | 0.035 (3) | 0.009 (2) | −0.009 (2) | −0.005 (2) |
C5 | 0.028 (2) | 0.031 (2) | 0.023 (2) | 0.0040 (18) | −0.0120 (18) | −0.0007 (18) |
C6 | 0.026 (2) | 0.031 (2) | 0.024 (2) | 0.0019 (18) | −0.0104 (18) | −0.0001 (18) |
C7 | 0.029 (2) | 0.045 (3) | 0.037 (3) | −0.005 (2) | −0.014 (2) | −0.003 (2) |
C8 | 0.037 (3) | 0.055 (3) | 0.047 (3) | −0.008 (2) | −0.023 (2) | −0.005 (3) |
C9 | 0.058 (3) | 0.036 (3) | 0.035 (3) | −0.007 (2) | −0.026 (2) | −0.005 (2) |
C10 | 0.040 (3) | 0.027 (2) | 0.025 (2) | 0.0008 (19) | −0.013 (2) | −0.0017 (18) |
C11 | 0.048 (3) | 0.050 (3) | 0.035 (3) | 0.024 (3) | −0.007 (2) | −0.001 (3) |
C12 | 0.027 (2) | 0.027 (2) | 0.029 (2) | −0.0002 (18) | −0.0044 (19) | 0.0001 (18) |
C13 | 0.044 (3) | 0.036 (3) | 0.035 (3) | −0.008 (2) | −0.018 (2) | −0.002 (2) |
C14 | 0.028 (2) | 0.026 (2) | 0.031 (2) | 0.0051 (18) | −0.0133 (19) | −0.0055 (18) |
C15 | 0.030 (2) | 0.041 (3) | 0.037 (3) | −0.002 (2) | −0.005 (2) | −0.003 (2) |
C16 | 0.030 (2) | 0.027 (2) | 0.037 (3) | −0.0005 (19) | −0.014 (2) | −0.0039 (19) |
C17 | 0.056 (3) | 0.053 (3) | 0.038 (3) | 0.028 (3) | −0.017 (3) | −0.015 (3) |
C18 | 0.035 (3) | 0.033 (2) | 0.032 (2) | 0.004 (2) | −0.011 (2) | −0.006 (2) |
C19 | 0.082 (5) | 0.037 (3) | 0.036 (3) | −0.006 (3) | −0.001 (3) | −0.012 (2) |
C20 | 0.043 (3) | 0.034 (3) | 0.031 (2) | −0.003 (2) | −0.012 (2) | −0.007 (2) |
C21 | 0.028 (2) | 0.036 (3) | 0.040 (3) | 0.003 (2) | −0.011 (2) | −0.007 (2) |
C22 | 0.027 (2) | 0.027 (2) | 0.026 (2) | −0.0008 (18) | −0.0124 (18) | 0.0023 (18) |
C23 | 0.028 (2) | 0.054 (3) | 0.039 (3) | −0.011 (2) | −0.016 (2) | 0.005 (2) |
C24 | 0.028 (2) | 0.023 (2) | 0.037 (3) | −0.0013 (18) | −0.012 (2) | 0.0008 (19) |
N1 | 0.0266 (18) | 0.0249 (18) | 0.0256 (18) | 0.0033 (15) | −0.0107 (15) | −0.0021 (15) |
N2 | 0.0256 (18) | 0.0276 (19) | 0.0194 (17) | −0.0001 (15) | −0.0081 (14) | 0.0004 (14) |
O1 | 0.0280 (16) | 0.0364 (18) | 0.0259 (16) | 0.0104 (13) | −0.0095 (13) | −0.0036 (13) |
O2 | 0.0335 (17) | 0.0319 (17) | 0.0283 (17) | 0.0065 (14) | −0.0102 (14) | −0.0010 (13) |
O3 | 0.0309 (17) | 0.0386 (18) | 0.0335 (17) | −0.0029 (14) | −0.0111 (14) | −0.0120 (14) |
O4 | 0.0366 (19) | 0.058 (2) | 0.0352 (19) | −0.0107 (17) | −0.0165 (16) | 0.0068 (17) |
O5 | 0.0274 (18) | 0.073 (3) | 0.039 (2) | 0.0029 (17) | −0.0082 (16) | 0.0047 (19) |
O6 | 0.050 (2) | 0.047 (2) | 0.047 (2) | 0.0044 (17) | −0.0269 (18) | −0.0088 (17) |
O7 | 0.0387 (19) | 0.051 (2) | 0.0352 (18) | 0.0203 (17) | −0.0163 (15) | −0.0184 (16) |
O8 | 0.0328 (17) | 0.0426 (19) | 0.0363 (18) | 0.0130 (15) | −0.0137 (15) | −0.0164 (15) |
O9 | 0.066 (2) | 0.0370 (19) | 0.0316 (18) | −0.0085 (17) | −0.0092 (17) | −0.0125 (15) |
O10 | 0.064 (2) | 0.0292 (18) | 0.0376 (19) | −0.0118 (16) | −0.0207 (18) | −0.0017 (15) |
O11 | 0.0334 (17) | 0.0272 (16) | 0.0357 (18) | −0.0002 (13) | −0.0119 (14) | −0.0078 (14) |
O12 | 0.0315 (17) | 0.0300 (17) | 0.0366 (18) | 0.0046 (14) | −0.0081 (14) | −0.0102 (14) |
O13 | 0.0248 (15) | 0.0373 (18) | 0.0273 (16) | −0.0042 (13) | −0.0097 (13) | 0.0025 (13) |
O14 | 0.0367 (18) | 0.0313 (17) | 0.0299 (17) | −0.0090 (14) | −0.0115 (14) | 0.0018 (14) |
F1 | 0.0355 (18) | 0.080 (3) | 0.064 (2) | 0.0046 (17) | 0.0084 (16) | −0.001 (2) |
F2 | 0.082 (3) | 0.097 (3) | 0.061 (2) | 0.068 (2) | −0.021 (2) | −0.011 (2) |
F3 | 0.085 (3) | 0.055 (2) | 0.0394 (18) | 0.0247 (19) | −0.0071 (17) | −0.0181 (16) |
F4 | 0.061 (2) | 0.066 (2) | 0.0328 (16) | −0.0203 (17) | −0.0163 (15) | 0.0063 (15) |
F5 | 0.054 (2) | 0.067 (2) | 0.054 (2) | 0.0038 (16) | −0.0371 (17) | 0.0065 (17) |
F6 | 0.094 (3) | 0.050 (2) | 0.059 (2) | −0.0105 (19) | −0.034 (2) | −0.0236 (17) |
F7B | 0.0400 (13) | 0.059 (2) | 0.067 (2) | −0.0038 (14) | −0.0103 (14) | −0.0076 (15) |
F8B | 0.0400 (13) | 0.059 (2) | 0.067 (2) | −0.0038 (14) | −0.0103 (14) | −0.0076 (15) |
F9B | 0.0400 (13) | 0.059 (2) | 0.067 (2) | −0.0038 (14) | −0.0103 (14) | −0.0076 (15) |
F7A | 0.0400 (13) | 0.059 (2) | 0.067 (2) | −0.0038 (14) | −0.0103 (14) | −0.0076 (15) |
F8A | 0.0400 (13) | 0.059 (2) | 0.067 (2) | −0.0038 (14) | −0.0103 (14) | −0.0076 (15) |
F9A | 0.0400 (13) | 0.059 (2) | 0.067 (2) | −0.0038 (14) | −0.0103 (14) | −0.0076 (15) |
F10A | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F11A | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F12A | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F10B | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F11B | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F12B | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F10C | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F11C | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F12C | 0.069 (3) | 0.082 (3) | 0.043 (2) | 0.030 (2) | −0.025 (2) | −0.0246 (19) |
F13B | 0.100 (2) | 0.055 (2) | 0.0388 (15) | −0.0058 (18) | −0.0148 (15) | 0.0073 (15) |
F14B | 0.100 (2) | 0.055 (2) | 0.0388 (15) | −0.0058 (18) | −0.0148 (15) | 0.0073 (15) |
F15B | 0.100 (2) | 0.055 (2) | 0.0388 (15) | −0.0058 (18) | −0.0148 (15) | 0.0073 (15) |
F13A | 0.100 (2) | 0.055 (2) | 0.0388 (15) | −0.0058 (18) | −0.0148 (15) | 0.0073 (15) |
F14A | 0.100 (2) | 0.055 (2) | 0.0388 (15) | −0.0058 (18) | −0.0148 (15) | 0.0073 (15) |
F15A | 0.100 (2) | 0.055 (2) | 0.0388 (15) | −0.0058 (18) | −0.0148 (15) | 0.0073 (15) |
F16 | 0.0357 (17) | 0.102 (3) | 0.050 (2) | 0.0014 (18) | 0.0008 (15) | −0.023 (2) |
F17 | 0.0382 (17) | 0.059 (2) | 0.065 (2) | 0.0098 (15) | −0.0288 (16) | 0.0025 (17) |
F18 | 0.0377 (17) | 0.0452 (19) | 0.105 (3) | −0.0101 (14) | −0.0281 (19) | −0.0073 (19) |
F19 | 0.0286 (17) | 0.083 (3) | 0.100 (3) | 0.0053 (17) | −0.0149 (18) | −0.024 (2) |
F20 | 0.054 (2) | 0.086 (3) | 0.054 (2) | −0.0278 (18) | −0.0305 (17) | 0.0004 (18) |
F21 | 0.0496 (19) | 0.076 (2) | 0.055 (2) | −0.0338 (18) | −0.0228 (16) | 0.0268 (18) |
Pt1—N1 | 1.982 (4) | C12—O1 | 1.272 (5) |
Pt1—N2 | 1.985 (4) | C13—F6 | 1.320 (6) |
Pt1—O1 | 2.034 (3) | C13—F5 | 1.330 (6) |
Pt1—O13 | 2.038 (3) | C13—F4 | 1.336 (6) |
Pt1—Ag1 | 2.9315 (4) | C13—C14 | 1.538 (6) |
K1—O2 | 2.772 (3) | C14—O4 | 1.238 (6) |
K1—O3 | 2.718 (3) | C14—O3 | 1.243 (5) |
K1—O4i | 2.923 (4) | C15—F8A | 1.325 (4) |
K1—O7i | 2.738 (3) | C15—F7B | 1.330 (5) |
K1—O9i | 2.745 (4) | C15—F9A | 1.331 (4) |
K1—O11 | 2.829 (3) | C15—F9B | 1.331 (5) |
K1—F10Ai | 2.926 (7) | C15—F8B | 1.334 (5) |
K1—F10Bi | 2.950 (11) | C15—F7A | 1.337 (4) |
K1—F10Ci | 3.232 (17) | C15—C16 | 1.536 (6) |
Ag1—O5 | 2.230 (3) | C16—O5 | 1.230 (6) |
Ag1—O14 | 2.474 (3) | C16—O6 | 1.231 (6) |
Ag1—O2 | 2.490 (3) | C17—F11B | 1.316 (5) |
Ag1—O11 | 2.578 (3) | C17—F10C | 1.318 (5) |
Ag1—Ag2 | 3.3140 (5) | C17—F11C | 1.321 (5) |
Ag2—O9 | 2.215 (3) | C17—F12A | 1.326 (5) |
Ag2—O3 | 2.298 (3) | C17—F12B | 1.334 (5) |
Ag2—O11 | 2.379 (3) | C17—F10A | 1.334 (5) |
Ag2—O6 | 2.556 (4) | C17—F11A | 1.343 (5) |
Ag2—Ag3 | 2.9702 (5) | C17—F12C | 1.352 (5) |
Ag3—O12 | 2.337 (3) | C17—F10B | 1.354 (5) |
Ag3—O6 | 2.344 (4) | C17—C18 | 1.535 (7) |
Ag3—O10 | 2.405 (3) | C18—O8 | 1.235 (5) |
Ag3—O12ii | 2.573 (3) | C18—O7 | 1.244 (6) |
Ag3—O14ii | 2.584 (3) | C19—F14A | 1.310 (5) |
Ag4—O8iii | 2.181 (3) | C19—F15B | 1.317 (5) |
Ag4—O7 | 2.218 (3) | C19—F13B | 1.337 (5) |
Ag4—O4 | 2.436 (3) | C19—F15A | 1.340 (5) |
Ag4—Ag4iii | 2.8671 (7) | C19—F13A | 1.345 (5) |
C1—N1 | 1.331 (6) | C19—F14B | 1.357 (5) |
C1—C2 | 1.381 (7) | C19—C20 | 1.539 (7) |
C1—H1A | 0.9300 | C20—O10 | 1.228 (6) |
C2—C3 | 1.363 (8) | C20—O9 | 1.245 (6) |
C2—H2A | 0.9300 | C21—F18 | 1.317 (6) |
C3—C4 | 1.375 (7) | C21—F16 | 1.318 (6) |
C3—H3A | 0.9300 | C21—F17 | 1.342 (6) |
C4—C5 | 1.380 (6) | C21—C22 | 1.534 (6) |
C4—H4A | 0.9300 | C22—O12 | 1.236 (5) |
C5—N1 | 1.363 (6) | C22—O11 | 1.252 (5) |
C5—C6 | 1.465 (6) | C23—F21 | 1.316 (6) |
C6—N2 | 1.357 (6) | C23—F20 | 1.316 (6) |
C6—C7 | 1.385 (6) | C23—F19 | 1.328 (7) |
C7—C8 | 1.366 (8) | C23—C24 | 1.540 (6) |
C7—H7A | 0.9300 | C24—O14 | 1.217 (5) |
C8—C9 | 1.377 (8) | C24—O13 | 1.277 (5) |
C8—H8A | 0.9300 | O4—K1i | 2.923 (4) |
C9—C10 | 1.381 (7) | O7—K1i | 2.738 (3) |
C9—H9A | 0.9300 | O8—Ag4iii | 2.181 (3) |
C10—N2 | 1.336 (6) | O9—K1i | 2.745 (4) |
C10—H10A | 0.9300 | O12—Ag3ii | 2.573 (3) |
C11—F2 | 1.324 (6) | O14—Ag3ii | 2.584 (3) |
C11—F1 | 1.325 (7) | F10A—K1i | 2.926 (7) |
C11—F3 | 1.327 (7) | F10B—K1i | 2.950 (11) |
C11—C12 | 1.541 (7) | F10C—K1i | 3.232 (17) |
C12—O2 | 1.223 (5) | ||
N1—Pt1—N2 | 81.04 (15) | C9—C8—H8A | 120.2 |
N1—Pt1—O1 | 177.55 (13) | C8—C9—C10 | 119.2 (5) |
N2—Pt1—O1 | 97.16 (14) | C8—C9—H9A | 120.4 |
N1—Pt1—O13 | 98.17 (14) | C10—C9—H9A | 120.4 |
N2—Pt1—O13 | 177.49 (13) | N2—C10—C9 | 121.4 (5) |
O1—Pt1—O13 | 83.56 (13) | N2—C10—H10A | 119.3 |
N1—Pt1—Ag1 | 90.97 (10) | C9—C10—H10A | 119.3 |
N2—Pt1—Ag1 | 95.74 (10) | F2—C11—F1 | 108.3 (5) |
O1—Pt1—Ag1 | 90.87 (8) | F2—C11—F3 | 107.7 (5) |
O13—Pt1—Ag1 | 86.64 (8) | F1—C11—F3 | 107.8 (5) |
O3—K1—O7i | 150.09 (11) | F2—C11—C12 | 111.4 (4) |
O3—K1—O9i | 72.60 (11) | F1—C11—C12 | 109.9 (5) |
O7i—K1—O9i | 105.10 (12) | F3—C11—C12 | 111.7 (5) |
O3—K1—O2 | 78.09 (10) | O2—C12—O1 | 129.8 (4) |
O7i—K1—O2 | 128.61 (11) | O2—C12—C11 | 118.9 (4) |
O9i—K1—O2 | 108.54 (11) | O1—C12—C11 | 111.3 (4) |
O3—K1—O11 | 66.03 (9) | F6—C13—F5 | 106.9 (4) |
O7i—K1—O11 | 104.37 (10) | F6—C13—F4 | 107.2 (4) |
O9i—K1—O11 | 136.71 (11) | F5—C13—F4 | 107.3 (4) |
O2—K1—O11 | 75.30 (9) | F6—C13—C14 | 112.1 (4) |
O3—K1—O4i | 82.77 (10) | F5—C13—C14 | 110.2 (4) |
O7i—K1—O4i | 67.36 (10) | F4—C13—C14 | 112.8 (4) |
O9i—K1—O4i | 90.44 (11) | O4—C14—O3 | 129.1 (4) |
O2—K1—O4i | 147.23 (11) | O4—C14—C13 | 115.4 (4) |
O11—K1—O4i | 72.68 (11) | O3—C14—C13 | 115.5 (4) |
O3—K1—F10Ai | 143.6 (2) | F8A—C15—F7B | 83.3 (5) |
O7i—K1—F10Ai | 54.81 (14) | F8A—C15—F9A | 106.9 (5) |
O9i—K1—F10Ai | 73.9 (3) | F7B—C15—F9A | 127.9 (6) |
O2—K1—F10Ai | 99.6 (2) | F8A—C15—F9B | 121.7 (7) |
O11—K1—F10Ai | 149.3 (3) | F7B—C15—F9B | 107.8 (6) |
O4i—K1—F10Ai | 111.47 (19) | F7B—C15—F8B | 106.6 (6) |
O3—K1—F10Bi | 138.2 (2) | F9A—C15—F8B | 85.5 (5) |
O7i—K1—F10Bi | 54.23 (18) | F9B—C15—F8B | 105.0 (6) |
O9i—K1—F10Bi | 66.3 (2) | F8A—C15—F7A | 106.5 (4) |
O2—K1—F10Bi | 107.8 (3) | F9A—C15—F7A | 108.0 (5) |
O11—K1—F10Bi | 155.70 (19) | F9B—C15—F7A | 85.1 (5) |
O4i—K1—F10Bi | 104.2 (2) | F8B—C15—F7A | 126.6 (6) |
F10Ai—K1—F10Bi | 10.0 (3) | F8A—C15—C16 | 114.3 (4) |
O3—K1—F10Ci | 153.3 (3) | F7B—C15—C16 | 110.5 (5) |
O7i—K1—F10Ci | 51.7 (2) | F9A—C15—C16 | 110.8 (4) |
O9i—K1—F10Ci | 87.4 (4) | F9B—C15—C16 | 114.2 (6) |
O2—K1—F10Ci | 92.24 (16) | F8B—C15—C16 | 112.4 (6) |
O11—K1—F10Ci | 135.9 (4) | F7A—C15—C16 | 110.1 (4) |
O4i—K1—F10Ci | 115.69 (15) | O5—C16—O6 | 131.1 (5) |
O3—K1—Ag1 | 46.86 (7) | O5—C16—C15 | 113.7 (4) |
O7i—K1—Ag1 | 142.91 (8) | O6—C16—C15 | 115.1 (4) |
O9i—K1—Ag1 | 111.70 (9) | F11B—C17—F10C | 129.1 (9) |
O2—K1—Ag1 | 41.46 (6) | F10C—C17—F11C | 115.9 (8) |
O11—K1—Ag1 | 43.25 (6) | F11B—C17—F12A | 81.8 (7) |
O4i—K1—Ag1 | 107.11 (8) | F10C—C17—F12A | 80.1 (8) |
F10Ai—K1—Ag1 | 141.0 (2) | F11C—C17—F12A | 121.3 (8) |
F10Bi—K1—Ag1 | 148.6 (2) | F11B—C17—F12B | 111.6 (7) |
F10Ci—K1—Ag1 | 132.89 (17) | F10C—C17—F12B | 46.0 (9) |
O3—K1—Ag2i | 63.55 (7) | F11C—C17—F12B | 137.5 (9) |
O7i—K1—Ag2i | 96.84 (8) | F11B—C17—F10A | 115.6 (8) |
O9i—K1—Ag2i | 35.25 (7) | F11C—C17—F10A | 84.6 (8) |
O2—K1—Ag2i | 132.33 (7) | F12A—C17—F10A | 110.8 (5) |
O11—K1—Ag2i | 110.24 (7) | F12B—C17—F10A | 80.2 (7) |
O4i—K1—Ag2i | 56.33 (7) | F10C—C17—F11A | 131.6 (8) |
F10Ai—K1—Ag2i | 95.7 (3) | F12A—C17—F11A | 104.4 (5) |
F10Bi—K1—Ag2i | 85.9 (2) | F12B—C17—F11A | 131.8 (7) |
F10Ci—K1—Ag2i | 109.2 (3) | F10A—C17—F11A | 105.1 (6) |
Ag1—K1—Ag2i | 110.38 (3) | F11B—C17—F12C | 60.0 (9) |
O3—K1—Ag2 | 36.72 (7) | F10C—C17—F12C | 105.4 (8) |
O7i—K1—Ag2 | 118.53 (8) | F11C—C17—F12C | 102.9 (7) |
O9i—K1—Ag2 | 98.76 (8) | F12B—C17—F12C | 61.9 (9) |
O2—K1—Ag2 | 93.41 (7) | F10A—C17—F12C | 131.5 (8) |
O11—K1—Ag2 | 38.65 (6) | F11A—C17—F12C | 82.3 (8) |
O4i—K1—Ag2 | 56.57 (8) | F11B—C17—F10B | 103.3 (7) |
F10Ai—K1—Ag2 | 166.6 (2) | F10C—C17—F10B | 57.3 (11) |
F10Bi—K1—Ag2 | 156.9 (3) | F11C—C17—F10B | 65.5 (10) |
F10Ci—K1—Ag2 | 169.9 (3) | F12A—C17—F10B | 129.3 (7) |
Ag1—K1—Ag2 | 51.970 (15) | F12B—C17—F10B | 101.8 (7) |
Ag2i—K1—Ag2 | 72.78 (2) | F11A—C17—F10B | 87.6 (8) |
O5—Ag1—O14 | 124.99 (14) | F12C—C17—F10B | 143.1 (9) |
O5—Ag1—O2 | 141.28 (13) | F11B—C17—C18 | 118.2 (6) |
O14—Ag1—O2 | 80.29 (11) | F10C—C17—C18 | 112.8 (7) |
O5—Ag1—O11 | 125.17 (12) | F11C—C17—C18 | 111.6 (7) |
O14—Ag1—O11 | 79.09 (10) | F12A—C17—C18 | 111.8 (5) |
O2—Ag1—O11 | 84.91 (10) | F12B—C17—C18 | 110.8 (6) |
O5—Ag1—Pt1 | 87.19 (9) | F10A—C17—C18 | 114.2 (5) |
O14—Ag1—Pt1 | 74.04 (7) | F11A—C17—C18 | 109.9 (5) |
O2—Ag1—Pt1 | 71.18 (7) | F12C—C17—C18 | 107.3 (7) |
O11—Ag1—Pt1 | 146.44 (7) | F10B—C17—C18 | 109.5 (6) |
O5—Ag1—Ag2 | 82.91 (9) | O8—C18—O7 | 129.9 (5) |
O14—Ag1—Ag2 | 118.65 (7) | O8—C18—C17 | 115.2 (4) |
O2—Ag1—Ag2 | 112.13 (7) | O7—C18—C17 | 114.9 (4) |
O11—Ag1—Ag2 | 45.55 (7) | F14A—C19—F15B | 111.3 (9) |
Pt1—Ag1—Ag2 | 167.005 (15) | F14A—C19—F13B | 81.2 (6) |
O5—Ag1—K1 | 132.74 (11) | F15B—C19—F13B | 109.8 (6) |
O14—Ag1—K1 | 101.17 (8) | F14A—C19—F15A | 110.6 (6) |
O2—Ag1—K1 | 47.48 (7) | F13B—C19—F15A | 126.2 (6) |
O11—Ag1—K1 | 48.75 (7) | F14A—C19—F13A | 111.1 (5) |
Pt1—Ag1—K1 | 117.771 (19) | F15B—C19—F13A | 87.0 (6) |
Ag2—Ag1—K1 | 64.676 (17) | F15A—C19—F13A | 102.2 (5) |
O9—Ag2—O3 | 133.48 (12) | F15B—C19—F14B | 102.5 (7) |
O9—Ag2—O11 | 137.93 (13) | F13B—C19—F14B | 102.9 (6) |
O3—Ag2—O11 | 80.53 (11) | F15A—C19—F14B | 96.5 (7) |
O9—Ag2—O6 | 95.43 (13) | F13A—C19—F14B | 131.9 (6) |
O3—Ag2—O6 | 95.45 (12) | F14A—C19—C20 | 115.6 (5) |
O11—Ag2—O6 | 106.31 (12) | F15B—C19—C20 | 117.9 (6) |
O9—Ag2—Ag3 | 90.59 (9) | F13B—C19—C20 | 115.4 (5) |
O3—Ag2—Ag3 | 129.37 (8) | F15A—C19—C20 | 106.1 (5) |
O11—Ag2—Ag3 | 77.88 (8) | F13A—C19—C20 | 110.3 (4) |
O6—Ag2—Ag3 | 49.50 (8) | F14B—C19—C20 | 106.3 (5) |
O9—Ag2—Ag1 | 162.57 (10) | O10—C20—O9 | 130.5 (5) |
O3—Ag2—Ag1 | 55.10 (8) | O10—C20—C19 | 115.4 (4) |
O11—Ag2—Ag1 | 50.66 (8) | O9—C20—C19 | 114.1 (4) |
O6—Ag2—Ag1 | 67.42 (9) | F18—C21—F16 | 106.8 (4) |
Ag3—Ag2—Ag1 | 76.010 (14) | F18—C21—F17 | 107.3 (4) |
O9—Ag2—K1i | 45.67 (9) | F16—C21—F17 | 106.5 (4) |
O3—Ag2—K1i | 87.90 (8) | F18—C21—C22 | 114.0 (4) |
O11—Ag2—K1i | 152.19 (8) | F16—C21—C22 | 113.0 (4) |
O6—Ag2—K1i | 99.87 (9) | F17—C21—C22 | 108.9 (4) |
Ag3—Ag2—K1i | 127.79 (2) | O12—C22—O11 | 129.8 (4) |
Ag1—Ag2—K1i | 137.293 (19) | O12—C22—C21 | 116.5 (4) |
O9—Ag2—K1 | 134.06 (10) | O11—C22—C21 | 113.6 (4) |
O3—Ag2—K1 | 45.01 (8) | F21—C23—F20 | 107.5 (4) |
O11—Ag2—K1 | 47.96 (8) | F21—C23—F19 | 107.9 (5) |
O6—Ag2—K1 | 129.10 (9) | F20—C23—F19 | 106.5 (4) |
Ag3—Ag2—K1 | 124.95 (2) | F21—C23—C24 | 113.6 (4) |
Ag1—Ag2—K1 | 63.354 (17) | F20—C23—C24 | 112.3 (4) |
K1i—Ag2—K1 | 107.22 (2) | F19—C23—C24 | 108.7 (4) |
O12—Ag3—O6 | 122.40 (12) | O14—C24—O13 | 129.1 (4) |
O12—Ag3—O10 | 110.06 (12) | O14—C24—C23 | 118.8 (4) |
O6—Ag3—O10 | 93.80 (12) | O13—C24—C23 | 112.0 (4) |
O12—Ag3—O12ii | 82.14 (11) | C1—N1—C5 | 120.0 (4) |
O6—Ag3—O12ii | 100.62 (12) | C1—N1—Pt1 | 124.7 (3) |
O10—Ag3—O12ii | 152.04 (11) | C5—N1—Pt1 | 115.2 (3) |
O12—Ag3—O14ii | 104.20 (11) | C10—N2—C6 | 119.6 (4) |
O6—Ag3—O14ii | 132.21 (12) | C10—N2—Pt1 | 125.0 (3) |
O10—Ag3—O14ii | 78.46 (11) | C6—N2—Pt1 | 115.4 (3) |
O12ii—Ag3—O14ii | 74.09 (10) | C12—O1—Pt1 | 118.8 (3) |
O12—Ag3—Ag2 | 83.13 (8) | C12—O2—Ag1 | 123.8 (3) |
O6—Ag3—Ag2 | 56.01 (9) | C12—O2—K1 | 136.9 (3) |
O10—Ag3—Ag2 | 70.58 (8) | Ag1—O2—K1 | 91.06 (10) |
O12ii—Ag3—Ag2 | 137.12 (7) | C14—O3—Ag2 | 114.7 (3) |
O14ii—Ag3—Ag2 | 148.76 (7) | C14—O3—K1 | 135.9 (3) |
O8iii—Ag4—O7 | 157.85 (13) | Ag2—O3—K1 | 98.27 (11) |
O8iii—Ag4—O4 | 117.26 (12) | C14—O4—Ag4 | 126.1 (3) |
O7—Ag4—O4 | 84.82 (13) | C14—O4—K1i | 139.8 (3) |
O8iii—Ag4—Ag4iii | 80.91 (8) | Ag4—O4—K1i | 92.61 (11) |
O7—Ag4—Ag4iii | 81.33 (8) | C16—O5—Ag1 | 120.3 (3) |
O4—Ag4—Ag4iii | 144.66 (10) | C16—O6—Ag3 | 131.4 (3) |
O8iii—Ag4—K1i | 152.68 (8) | C16—O6—Ag2 | 122.2 (3) |
O7—Ag4—K1i | 43.33 (8) | Ag3—O6—Ag2 | 74.50 (10) |
O4—Ag4—K1i | 48.65 (8) | C18—O7—Ag4 | 120.4 (3) |
Ag4iii—Ag4—K1i | 124.59 (2) | C18—O7—K1i | 132.1 (3) |
N1—C1—C2 | 121.0 (5) | Ag4—O7—K1i | 102.90 (12) |
N1—C1—H1A | 119.5 | C18—O8—Ag4iii | 123.3 (3) |
C2—C1—H1A | 119.5 | C20—O9—Ag2 | 113.8 (3) |
C3—C2—C1 | 119.8 (5) | C20—O9—K1i | 143.3 (3) |
C3—C2—H2A | 120.1 | Ag2—O9—K1i | 99.08 (12) |
C1—C2—H2A | 120.1 | C20—O10—Ag3 | 131.0 (3) |
C2—C3—C4 | 119.3 (5) | C22—O11—Ag2 | 121.9 (3) |
C2—C3—H3A | 120.4 | C22—O11—Ag1 | 108.9 (3) |
C4—C3—H3A | 120.4 | Ag2—O11—Ag1 | 83.80 (10) |
C3—C4—C5 | 119.6 (5) | C22—O11—K1 | 141.6 (3) |
C3—C4—H4A | 120.2 | Ag2—O11—K1 | 93.39 (10) |
C5—C4—H4A | 120.2 | Ag1—O11—K1 | 88.00 (9) |
N1—C5—C4 | 120.2 (4) | C22—O12—Ag3 | 120.1 (3) |
N1—C5—C6 | 114.1 (4) | C22—O12—Ag3ii | 119.8 (3) |
C4—C5—C6 | 125.6 (4) | Ag3—O12—Ag3ii | 97.86 (11) |
N2—C6—C7 | 120.8 (4) | C24—O13—Pt1 | 123.9 (3) |
N2—C6—C5 | 114.2 (4) | C24—O14—Ag1 | 116.9 (3) |
C7—C6—C5 | 125.0 (4) | C24—O14—Ag3ii | 122.3 (3) |
C8—C7—C6 | 119.3 (5) | Ag1—O14—Ag3ii | 115.14 (12) |
C8—C7—H7A | 120.4 | C17—F10A—K1i | 122.4 (5) |
C6—C7—H7A | 120.4 | C17—F10B—K1i | 119.9 (7) |
C7—C8—C9 | 119.7 (5) | C17—F10C—K1i | 106.0 (9) |
C7—C8—H8A | 120.2 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | K2[Pt2Ag8(C10H8N2)2(C2F3O2)14] |
Mr | 3225.98 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 11.9829 (6), 12.4737 (6), 14.4368 (7) |
α, β, γ (°) | 77.378 (1), 70.132 (1), 86.305 (1) |
V (Å3) | 1980.28 (17) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 5.73 |
Crystal size (mm) | 0.10 × 0.10 × 0.05 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2008) |
Tmin, Tmax | 0.598, 0.763 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20732, 7748, 7189 |
Rint | 0.018 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.058, 1.03 |
No. of reflections | 7748 |
No. of parameters | 609 |
No. of restraints | 112 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.97, −1.24 |
Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al., 2006), SHELXTL (Sheldrick, 2008).
Pt1—Ag1 | 2.9314 (3) | Pt1···Pt1A | 3.4804 (3) |
Ag1—Ag2 | 3.3140 (5) | Ag3···Ag3A | 3.7053 (7) |
Ag2—Ag3 | 2.9702 (5) | Ag4—Ag4A | 2.8671 (7) |
Ag3—O6 | 2.345 (3) | Ag3—O12A | 2.572 (3) |
Pt—O1 | 2.033 (3) | K1—O2 | 2.771 (3) |
Pt1—O13 | 2.038 (3) | K1—O3 | 2.717 (3) |
Pt1—N1 | 1.981 (3) | K1—O11 | 2.829 (3) |
Pt1—N2 | 1.985 (3) | ||
O1—Pt1—O13 | 83.5 (1) | N1—Pt1—N2 | 81.0 (1) |
O1—Pt1—N2 | 97.2 (1) | O13—Pt1—N1 | 98.2 (1) |
O2—Ag1—O5 | 141.2 (1) | O2—Ag1—O14 | 80.38 (9) |
O5—Ag1—O14 | 124.9 (1) | Pt1—Ag1—Ag2 | 167.00 (1) |
Ag1—Ag2—Ag3 | 76.01 (1) |
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Coordination polymers are of current interest in materials science due to their potential applications as, for example, luminescent materials (Brandys & Puddephatt, 2001; Shyu et al., 2009), catalysts (Bordoloi et al., 2007) and materials for hydrogen storage (Jeon et al., 2008). Nonetheless, controlling the chemical structure of extended heterometallic networks remains a challenge. Aggregates of Ag(O2CR) are well documented in the literature, and are known to form [Ag(O2CR)]n aggregates via bridging carboxylate moieties (see, for example, Karpova et al., 1999; Zhao et al., 2003; Zhao & Mak, 2005). We have recently reported the synthesis and structural characterization of several bimetallic complexes with the AgI:PtII ratio ranging from 1:1 to 3:1, in which Pt(2,2'-bipy) acts as a terminator for aggregates of Ag(O2CCF3) (Sun et al., 2009). Therein we have demonstrated that by controlling the stoichiometry of the reaction between Pt(2,2'-bipy)(O2CCF3)2 and Ag(O2CCF3), bimetallic structures with well defined geometries may be synthesized reproducibly.
Notably, none of the previously reported Pt(bipy)–Ag(O2CCF3) bimetallic complexes form extended one- or two-dimensional structures via the carboxylate bridging ligand, due to the terminating effect of the Pt(bipy) group. Instead, they form one-dimensional extended structures via intramolecular Pt···Pt interactions. In addition, despite the use of large excesses of Ag(O2CCF3) relative to PtII, complexes with an Ag:Pt ratio greater than 3:1 were not achieved. We have since discovered the title compound, (I), with the formula K2[Pt2Ag8(2,2'-bipy)2(O2CCF3)14], obtained serendipitously from the reaction of Pt(2,2'-bipy)(O2CCF3)2 with Ag(O2CCF3) in the presence of KCl. We have found that the presence of K+ ions drastically alters the crystal structure of the coordination polymer, forming structures that are extended in three dimensions as opposed to only one. The repeat unit of (I) is illustrated in the scheme, and consists of two asymmetric units of K[PtAg4(bipy)(O2CCF3)7] related by an inversion centre.
The structure of the asymmetric unit is shown in Fig. 1, where the PtII centre is in a typical square-planar environment, with normal Pt—O and Pt—N bond lengths. However, the O1—Pt1—O13 and N1—Pt1—N2 bond angles [83.5 (1) and 81.0 (1)°, respectively] do show significant deviation from an ideal square-planar geometry. The Ag4···Ag4A separation distance of 2.8671 (7) Å is approximately equal to the Ag—Ag distance in metallic silver (2.889 Å; Emsley, 1991), indicative of metal–metal bonding interactions. Meanwhile, the Ag1···Ag2 and Ag2···Ag3 distances are 3.3140 (5) and 2.9702 (5) Å, respectively, and thus represent only weak interactions between these metal centres. The coordination numbers around the AgI centres vary considerably, with Ag1 and Ag2 in distorted tetrahedral geometries, Ag3 in a distorted trigonal–bipyramidal geometry, and Ag4 adopting a distorted trigonal-planar geometry.
In the repeat unit of the [Pt2Ag8(2,2'-bipy)2(O2CCF3)14]2- anion of (I), six AgI ions and two PtII ions are joined together by ten carboxylate ligands, as shown in Fig. 2(a). Four of the ten carboxylate ligands adopt a µ2,η2-bridging mode, four adopt a µ3,η2-bridging mode and the remaining two adopt an uncommon µ4,η2-bridging mode. This Pt2Ag6 unit is quite different from the neutral Pt2Ag6(bipy)2(O2CCF3)10 complex, (II), which we reported earlier (Sun et al., 2009), in terms of the Ag6 arrangement and carboxylate coordination modes. In (II), four carboxylates act as µ3,η2-bridging ligands while the rest are µ2,η2-type ligands. Interestingly, the Pt2Ag6 unit in (I) is further linked to an Ag2(O2CCF3)2 unit via a µ2,η2-carboxylate group that binds to Ag3 and Ag4A, forming an extended one-dimensional coordination polymer, as shown in Fig. 2(b). This extra µ2,η2-carboxylate associated with the K+ cation thus allows the anionic cluster to form extended structures with a Pt:Ag ratio of 1:4.
Neighbouring polymer chains in this system are held together by two distinct interactions. First, chains stack on top of one another via attractive Pt···Pt interactions, in a similar manner to those observed previously by our group (Sun et al., 2009). The Pt···Pt separation distance in this case is 3.4804 (3) Å, which is typical of previously reported one-dimensional PtII chains (Du et al., 2008; Wadas et al., 2004). These interactions are shown in Fig. 3. In addition, electrostatic interactions with K+ ions join adjacent chains together in a direction perpendicular to the 110 plane, as shown in Fig. 4. These K+ ions are found in an octahedral coordination environment, depicted in Fig. 5.
In summary, we have reported a unique PtII–AgI coordination polymer supported by -O2CCF3 bridging ligands and K+ ions. We have also demonstrated that the presence of K+ ions has a significant impact on the formation of PtII–AgI heterometallic complexes. While previously reported complexes of this type form linear chains, the introduction of K+ causes these compounds to exhibit long-range order in three dimensions. Future avenues for research include the use of alternative cations to synthesize a wider variety of coordination polymers and metal–organic frameworks.