The syntheses and structures of two mixed-ligand complexes of platinum(II) with deprotonated oxopurine bases and triphenylphosphine are reported, namely the theophyllinate complex cis-bis(1,2,3,6-tetrahydro-1,3-dimethylpurine-2,6-dionato-κN7)bis(triphenylphosphine-κP)platinum(II), [Pt(C7H7N4O2)2(C18H15P)2], (I), and the theobrominate complex cis-chloro(1,2,3,6-tetrahydro-3,7-dimethylpurine-2,6-dionato-κN1)bis(triphenylphosphine-κP)platinum(II) ethanol hemisolvate, [PtCl(C7H7N4O2)(C18H15P)2]·0.5C2H5OH, (II). In (I), the coordination geometry of Pt is square planar, formed by the two coordinating N atoms of the theophyllinate anions in a cis arrangement and two P atoms from the triphenylphosphine groups. In (II), there are two crystallographically independent molecules. They both exhibit a square-planar coordination geometry around Pt involving one Cl atom, the coordinating N atom of the theobrominate anion and two P atoms from the triphenylphosphine groups. The two triphenylphosphine groups are arranged in a cis configuration in both structures. The heterocyclic rings are rotated with respect to the coordination plane of the metal by 82.99 (8) and 88.09 (8)° in complex (I), and by 85.91 (16) and 88.14 (18)° in complex (II). Both structures are stabilized by intramolecular stacking interactions involving the purine rings and the phenyl rings of adjacent triphenylphosphine moieties.
Supporting information
CCDC references: 181997; 181998
Complex (I) was crystallized by adding a suspension of
cis-[PtCl2(PPh3)2] (119 mg, 0.15 mmol) in ethanol (50 ml) to a
solution of theophylline (54 mg, 0.3 mmol) in water (5 ml) containing NaOH
(0.3 mmol). The reaction mixture was heated to give a clear solution. After
slow evaporation at room temperature for one month, colourless plates of (I)
were formed. Elemental analysis: found: C 55.40, H 4.27, N 9.99%; calculated
for C50H44N8O4P2Pt: C 55.71, H 4.11, N 10.39%. A molecular peak
corresponding to [Pt(TP-)2(PPh3)2]H+ at m/z 1078 (2%) and a
peak corresponding to [Pt(TP-)(PPh3)2]+ at m/z 898 (43%) were
found in the FAB-MS. Complex (II) was obtained by adding a suspension of
cis-[PtCl2(PPh3)2] (119 mg; 0.15 mmol) in ethanol (50 ml) to a
solution of theobromine (27 mg, 0.15 mmol) in water (5 ml) containing NaOH
(0.3 mmol). The reaction mixture was heated to give a clear solution. After
slow evaporation at room temperature for one month at 323 K Please clarify
which temperature applied and subsequent slow addition of a solution of an
excess of NaBF4 in 100 µl of the main solution, colourless plates of (II)
formed. Elemental analysis: found: C 54.93, H 3.99, N 5.83%, calculated for
C44H40ClN4O2.5P2Pt: C 55.20, H 4.21, N 5.85%. A molecular peak
corresponding to [Pt(TB-)(PPh3)2]+ at m/z 898 (67%) and a peak
corresponding to [PtCl(TB-)(PPh3)2]Na+ at m/z 957 (4%) were
found in the FAB-MS.
The abnormalities of the displacement parameters of N72 in (I) may be related to
systematic errors that probably occurred during the indexing of crystal faces
and measurement of the face-to-face distances of the tiny crystal with the aid
of a video camera. Four anisotropic displacement parameters of (II) showed
max/min ratios larger than 3.0, with a maximum value of 3.70 for atom C3H.
This may be explained by the low diffraction power and small size of the
crystal used, resulting in only 44% observed reflections. For the phenyl rings
of (II), rigid group constraints (AFIX 66 in SHELXL97; Sheldrick, 1997)
were used. Ten 1,2- and two 1,3-distance restraints (DFIX) were applied
for the purine ring system of molecule 1. Similarity restraints were used for
the purine ring system of molecule 2 with the SAME instruction. The solvent
ethanol of (II) appeared to be disordered, with very large displacement
parameters. Therefore, the site occupancy was started at 0.5 and the atoms
were refined with the PART instruction. The isotropic displacement parameters
of the corresponding C and O atoms were equated by using EADP constraints. The
1,2- and 1,3- distance restraints which were applied for the ethanol molecules
were based on theoretical calculations. Attempts to localize the hydroxy H
atoms H5 and H6 using AFIX 87/AFIX 83 options, and also using extended
difference electron density calculations that could lead to the expected
hydrogen-bonding contacts, were unsuccessful. Therefore, the calculated
positions of H5 and H6 (AFIX 83) were used as a starting set for restraint
models of O5—H5···O61 and O6—H6···O21 hydrogen contacts by using 1,2- and
1,3-distance restraints (DFIX). Many cycles of refinement were
necessary for convergence, using the shift-limiting DAMP option. The last
cycle of refinement was calculated separately with DAMP 0 0 to obtain the
correct standard uncertainties. The final disorder ratio of the ethanol
molecules was 60:40. A l l H-atom positions were calculated [except H5 and H6
in (II)] after each cycle of refinement with SHELXL97, using a riding
model in both structures, with C—H = 0.95–0.99 Å and Uiso(H) =
1.5Ueq(C). Are these the correct constraints?
For both compounds, data collection: IPDS (Stoe & Cie, 1999); cell refinement: IPDS; data reduction: X-RED in IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1990) and PLUTON (Spek, 1997); software used to prepare material for publication: SHELXL97.
(I)
cis-bis(1,2,3,6-tetrahydro-1,3-dimethylpurine-2,6-dionato-
κN7)bis (triphenylphosphine-
κP)platinum(II)
top
Crystal data top
[Pt(C7H7N4O2)2(C18H15P)2] | F(000) = 2160 |
Mr = 1077.96 | Dx = 1.614 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.7839 (5) Å | Cell parameters from 8000 reflections |
b = 20.7991 (10) Å | θ = 2.7–30.3° |
c = 22.0788 (12) Å | µ = 3.29 mm−1 |
β = 99.172 (6)° | T = 183 K |
V = 4435.5 (4) Å3 | Plate, colourless |
Z = 4 | 0.27 × 0.16 × 0.08 mm |
Data collection top
Stoe IPDS diffractometer | 13203 independent reflections |
Radiation source: fine-focus sealed tube | 9092 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.067 |
ϕ rotation scan | θmax = 30.3°, θmin = 2.6° |
Absorption correction: numerical (Coppens et al., 1965) | h = −13→13 |
Tmin = 0.470, Tmax = 0.779 | k = 0→29 |
52916 measured reflections | l = 0→31 |
Refinement top
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.084 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.038P)2] where P = (Fo2 + 2Fc2)/3 |
13203 reflections | (Δ/σ)max = 0.003 |
585 parameters | Δρmax = 1.42 e Å−3 |
0 restraints | Δρmin = −3.35 e Å−3 |
Crystal data top
[Pt(C7H7N4O2)2(C18H15P)2] | V = 4435.5 (4) Å3 |
Mr = 1077.96 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.7839 (5) Å | µ = 3.29 mm−1 |
b = 20.7991 (10) Å | T = 183 K |
c = 22.0788 (12) Å | 0.27 × 0.16 × 0.08 mm |
β = 99.172 (6)° | |
Data collection top
Stoe IPDS diffractometer | 13203 independent reflections |
Absorption correction: numerical (Coppens et al., 1965) | 9092 reflections with I > 2σ(I) |
Tmin = 0.470, Tmax = 0.779 | Rint = 0.067 |
52916 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.084 | H-atom parameters constrained |
S = 1.01 | Δρmax = 1.42 e Å−3 |
13203 reflections | Δρmin = −3.35 e Å−3 |
585 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pt | 0.492780 (15) | 0.104579 (7) | 0.766770 (7) | 0.00969 (4) | |
P1 | 0.47785 (10) | 0.01295 (5) | 0.70948 (5) | 0.01226 (19) | |
P2 | 0.51296 (10) | 0.05731 (5) | 0.86037 (5) | 0.01129 (19) | |
N11 | 0.0980 (4) | 0.1898 (2) | 0.62549 (19) | 0.0309 (10) | |
C11 | −0.0460 (6) | 0.1860 (4) | 0.6374 (3) | 0.0522 (19) | |
H11A | −0.0853 | 0.2294 | 0.6370 | 0.078* | |
H11B | −0.0472 | 0.1663 | 0.6776 | 0.078* | |
H11C | −0.1012 | 0.1599 | 0.6056 | 0.078* | |
C21 | 0.1151 (5) | 0.2116 (3) | 0.5671 (2) | 0.0285 (11) | |
O21 | 0.0151 (4) | 0.2281 (2) | 0.52972 (18) | 0.0455 (11) | |
N31 | 0.2479 (4) | 0.2149 (2) | 0.55393 (18) | 0.0252 (9) | |
C31 | 0.2669 (6) | 0.2317 (3) | 0.4915 (2) | 0.0373 (13) | |
H31A | 0.1994 | 0.2082 | 0.4621 | 0.056* | |
H31B | 0.3608 | 0.2201 | 0.4854 | 0.056* | |
H31C | 0.2531 | 0.2780 | 0.4852 | 0.056* | |
C41 | 0.3580 (5) | 0.1959 (2) | 0.5981 (2) | 0.0195 (9) | |
C51 | 0.3365 (5) | 0.1725 (2) | 0.6542 (2) | 0.0183 (9) | |
C61 | 0.2039 (5) | 0.1672 (3) | 0.6716 (2) | 0.0249 (10) | |
O61 | 0.1749 (4) | 0.1462 (2) | 0.72023 (17) | 0.0416 (11) | |
N71 | 0.4672 (4) | 0.15560 (16) | 0.68528 (15) | 0.0134 (7) | |
C81 | 0.5517 (5) | 0.1711 (2) | 0.6469 (2) | 0.0234 (10) | |
H81 | 0.6489 | 0.1648 | 0.6568 | 0.028* | |
N91 | 0.4935 (4) | 0.1961 (2) | 0.59291 (18) | 0.0256 (9) | |
N12 | 0.8715 (4) | 0.2562 (2) | 0.8392 (2) | 0.0266 (9) | |
C12 | 1.0126 (6) | 0.2507 (3) | 0.8234 (3) | 0.0450 (16) | |
H12A | 1.0390 | 0.2917 | 0.8066 | 0.068* | |
H12B | 1.0138 | 0.2168 | 0.7927 | 0.068* | |
H12C | 1.0783 | 0.2401 | 0.8603 | 0.068* | |
C22 | 0.8507 (5) | 0.3065 (3) | 0.8789 (2) | 0.0273 (10) | |
O22 | 0.9457 (4) | 0.34290 (19) | 0.89915 (18) | 0.0374 (9) | |
N32 | 0.7205 (4) | 0.3135 (2) | 0.89389 (18) | 0.0237 (8) | |
C32 | 0.6996 (6) | 0.3591 (3) | 0.9419 (3) | 0.0337 (12) | |
H32A | 0.7779 | 0.3566 | 0.9755 | 0.051* | |
H32B | 0.6139 | 0.3485 | 0.9573 | 0.051* | |
H32C | 0.6930 | 0.4027 | 0.9249 | 0.051* | |
C42 | 0.6158 (5) | 0.2724 (2) | 0.8673 (2) | 0.0187 (9) | |
C52 | 0.6401 (4) | 0.2229 (2) | 0.82945 (19) | 0.0173 (8) | |
C62 | 0.7725 (5) | 0.2106 (2) | 0.8130 (2) | 0.0231 (10) | |
O62 | 0.8042 (4) | 0.16728 (19) | 0.77986 (18) | 0.0331 (9) | |
N72 | 0.5137 (4) | 0.19255 (17) | 0.81127 (16) | 0.0153 (7) | |
C82 | 0.4243 (5) | 0.2256 (2) | 0.8383 (2) | 0.0198 (9) | |
H82 | 0.3287 | 0.2149 | 0.8336 | 0.024* | |
N92 | 0.4805 (4) | 0.27633 (19) | 0.87368 (19) | 0.0237 (8) | |
C1A | 0.3700 (4) | 0.0232 (2) | 0.63382 (19) | 0.0160 (9) | |
C2A | 0.2257 (5) | 0.0219 (3) | 0.6275 (2) | 0.0265 (11) | |
H2A | 0.1825 | 0.0124 | 0.6621 | 0.032* | |
C3A | 0.1442 (5) | 0.0346 (3) | 0.5709 (3) | 0.0365 (13) | |
H3A | 0.0462 | 0.0334 | 0.5670 | 0.044* | |
C4A | 0.2057 (6) | 0.0487 (3) | 0.5206 (2) | 0.0333 (12) | |
H4A | 0.1502 | 0.0580 | 0.4823 | 0.040* | |
C5A | 0.3482 (6) | 0.0494 (3) | 0.5260 (2) | 0.0298 (11) | |
H5A | 0.3905 | 0.0583 | 0.4911 | 0.036* | |
C6A | 0.4311 (5) | 0.0371 (2) | 0.5829 (2) | 0.0207 (9) | |
H6A | 0.5291 | 0.0383 | 0.5864 | 0.025* | |
C7A | 0.6449 (4) | −0.0098 (2) | 0.69008 (18) | 0.0129 (7)* | |
C8A | 0.6585 (5) | −0.0664 (2) | 0.65598 (19) | 0.0190 (9) | |
H8A | 0.5799 | −0.0923 | 0.6419 | 0.023* | |
C9A | 0.7885 (5) | −0.0835 (2) | 0.6434 (2) | 0.0240 (10) | |
H9A | 0.7989 | −0.1217 | 0.6211 | 0.029* | |
C10A | 0.9032 (5) | −0.0453 (3) | 0.6632 (2) | 0.0277 (11) | |
H10A | 0.9919 | −0.0583 | 0.6554 | 0.033* | |
C11A | 0.8890 (5) | 0.0115 (3) | 0.6941 (2) | 0.0284 (11) | |
H11D | 0.9670 | 0.0386 | 0.7059 | 0.034* | |
C12A | 0.7600 (4) | 0.0290 (2) | 0.7077 (2) | 0.0184 (9) | |
H12D | 0.7505 | 0.0678 | 0.7293 | 0.022* | |
C13A | 0.4073 (4) | −0.0580 (2) | 0.74225 (19) | 0.0162 (8) | |
C14A | 0.4776 (5) | −0.1166 (2) | 0.7518 (2) | 0.0244 (10) | |
H14A | 0.5663 | −0.1212 | 0.7399 | 0.029* | |
C15A | 0.4189 (6) | −0.1681 (3) | 0.7785 (2) | 0.0343 (12) | |
H15A | 0.4678 | −0.2077 | 0.7847 | 0.041* | |
C16A | 0.2902 (7) | −0.1624 (3) | 0.7961 (3) | 0.0393 (14) | |
H16A | 0.2499 | −0.1981 | 0.8135 | 0.047* | |
C17A | 0.2208 (6) | −0.1052 (3) | 0.7886 (3) | 0.0388 (13) | |
H17A | 0.1329 | −0.1012 | 0.8013 | 0.047* | |
C18A | 0.2784 (5) | −0.0522 (3) | 0.7620 (2) | 0.0241 (10) | |
H18A | 0.2300 | −0.0125 | 0.7575 | 0.029* | |
C1B | 0.6088 (4) | 0.1070 (2) | 0.92163 (16) | 0.0136 (7) | |
C2B | 0.5419 (5) | 0.1395 (2) | 0.9634 (2) | 0.0257 (10) | |
H2B | 0.4448 | 0.1350 | 0.9617 | 0.031* | |
C3B | 0.6172 (6) | 0.1789 (3) | 1.0078 (3) | 0.0399 (14) | |
H3B | 0.5710 | 0.2008 | 1.0364 | 0.048* | |
C4B | 0.7569 (6) | 0.1863 (3) | 1.0106 (2) | 0.0330 (12) | |
H4B | 0.8073 | 0.2130 | 1.0412 | 0.040* | |
C5B | 0.8249 (5) | 0.1551 (3) | 0.9690 (2) | 0.0303 (11) | |
H5B | 0.9219 | 0.1604 | 0.9708 | 0.036* | |
C6B | 0.7513 (4) | 0.1159 (2) | 0.9248 (2) | 0.0245 (11) | |
H6B | 0.7984 | 0.0948 | 0.8960 | 0.029* | |
C7B | 0.3443 (4) | 0.0464 (2) | 0.88520 (19) | 0.0155 (8) | |
C8B | 0.3306 (5) | 0.0168 (3) | 0.9403 (2) | 0.0231 (10) | |
H8B | 0.4096 | −0.0014 | 0.9649 | 0.028* | |
C9B | 0.2028 (5) | 0.0135 (3) | 0.9596 (2) | 0.0328 (12) | |
H9B | 0.1939 | −0.0067 | 0.9973 | 0.039* | |
C10B | 0.0881 (5) | 0.0401 (3) | 0.9232 (3) | 0.0384 (14) | |
H10B | 0.0000 | 0.0371 | 0.9359 | 0.046* | |
C11B | 0.0998 (5) | 0.0710 (3) | 0.8686 (2) | 0.0313 (12) | |
H11E | 0.0208 | 0.0899 | 0.8446 | 0.038* | |
C12B | 0.2283 (4) | 0.0741 (2) | 0.8496 (2) | 0.0193 (9) | |
H12E | 0.2373 | 0.0951 | 0.8122 | 0.023* | |
C13B | 0.6096 (4) | −0.0186 (2) | 0.86916 (19) | 0.0153 (8) | |
C14B | 0.7365 (5) | −0.0184 (3) | 0.8480 (2) | 0.0267 (10) | |
H14B | 0.7652 | 0.0190 | 0.8288 | 0.032* | |
C15B | 0.8216 (6) | −0.0726 (3) | 0.8549 (3) | 0.0418 (15) | |
H15B | 0.9084 | −0.0722 | 0.8408 | 0.050* | |
C16B | 0.7781 (7) | −0.1268 (3) | 0.8825 (3) | 0.0463 (16) | |
H16B | 0.8362 | −0.1636 | 0.8882 | 0.056* | |
C17B | 0.6516 (7) | −0.1278 (3) | 0.9019 (3) | 0.0378 (13) | |
H17B | 0.6216 | −0.1657 | 0.9198 | 0.045* | |
C18B | 0.5667 (5) | −0.0737 (2) | 0.8954 (2) | 0.0247 (10) | |
H18B | 0.4794 | −0.0748 | 0.9091 | 0.030* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pt | 0.00817 (6) | 0.01008 (6) | 0.01113 (6) | 0.00007 (7) | 0.00244 (4) | 0.00021 (7) |
P1 | 0.0104 (4) | 0.0142 (5) | 0.0129 (5) | −0.0010 (4) | 0.0042 (4) | −0.0010 (4) |
P2 | 0.0088 (4) | 0.0129 (5) | 0.0122 (5) | −0.0007 (4) | 0.0019 (3) | −0.0017 (4) |
N11 | 0.025 (2) | 0.044 (3) | 0.024 (2) | 0.015 (2) | 0.0041 (16) | 0.012 (2) |
C11 | 0.024 (3) | 0.089 (5) | 0.044 (3) | 0.025 (3) | 0.008 (2) | 0.025 (4) |
C21 | 0.033 (3) | 0.028 (3) | 0.023 (2) | 0.016 (2) | −0.001 (2) | 0.001 (2) |
O21 | 0.040 (2) | 0.062 (3) | 0.031 (2) | 0.025 (2) | −0.0045 (17) | 0.012 (2) |
N31 | 0.033 (2) | 0.024 (2) | 0.0163 (18) | 0.0077 (18) | −0.0009 (16) | 0.0046 (16) |
C31 | 0.053 (4) | 0.039 (3) | 0.019 (2) | 0.003 (3) | 0.003 (2) | 0.007 (2) |
C41 | 0.026 (2) | 0.018 (2) | 0.014 (2) | 0.0003 (18) | 0.0037 (17) | 0.0036 (17) |
C51 | 0.024 (2) | 0.015 (2) | 0.017 (2) | 0.0052 (17) | 0.0057 (17) | 0.0028 (16) |
C61 | 0.023 (2) | 0.030 (3) | 0.021 (2) | 0.012 (2) | 0.0031 (18) | 0.006 (2) |
O61 | 0.0265 (19) | 0.070 (3) | 0.031 (2) | 0.0166 (19) | 0.0130 (16) | 0.026 (2) |
N71 | 0.0211 (17) | 0.0099 (16) | 0.0082 (15) | 0.0045 (13) | −0.0008 (13) | 0.0021 (13) |
C81 | 0.022 (2) | 0.018 (2) | 0.029 (2) | 0.0001 (18) | 0.0006 (18) | 0.0034 (19) |
N91 | 0.029 (2) | 0.028 (2) | 0.0204 (19) | −0.0045 (18) | 0.0069 (16) | 0.0083 (17) |
N12 | 0.0219 (19) | 0.027 (2) | 0.032 (2) | −0.0094 (17) | 0.0068 (17) | −0.0060 (18) |
C12 | 0.024 (3) | 0.056 (4) | 0.058 (4) | −0.013 (3) | 0.015 (3) | −0.012 (3) |
C22 | 0.031 (3) | 0.024 (3) | 0.026 (2) | −0.010 (2) | 0.000 (2) | 0.002 (2) |
O22 | 0.038 (2) | 0.033 (2) | 0.040 (2) | −0.0209 (17) | 0.0006 (17) | −0.0058 (18) |
N32 | 0.029 (2) | 0.0166 (19) | 0.024 (2) | −0.0063 (17) | 0.0019 (16) | −0.0050 (16) |
C32 | 0.042 (3) | 0.024 (3) | 0.034 (3) | −0.001 (2) | 0.000 (2) | −0.010 (2) |
C42 | 0.027 (2) | 0.011 (2) | 0.018 (2) | −0.0039 (17) | 0.0030 (18) | −0.0008 (17) |
C52 | 0.020 (2) | 0.017 (2) | 0.0154 (19) | −0.0016 (17) | 0.0058 (16) | 0.0003 (16) |
C62 | 0.019 (2) | 0.024 (2) | 0.027 (2) | −0.0083 (18) | 0.0039 (18) | −0.0025 (19) |
O62 | 0.0235 (18) | 0.032 (2) | 0.046 (2) | −0.0051 (15) | 0.0129 (16) | −0.0201 (18) |
N72 | 0.0176 (17) | 0.0095 (16) | 0.0176 (17) | −0.0056 (13) | −0.0007 (13) | −0.0087 (13) |
C82 | 0.023 (2) | 0.016 (2) | 0.021 (2) | −0.0021 (17) | 0.0047 (17) | −0.0104 (17) |
N92 | 0.027 (2) | 0.0148 (19) | 0.030 (2) | −0.0005 (16) | 0.0061 (17) | −0.0073 (16) |
C1A | 0.017 (2) | 0.018 (2) | 0.012 (2) | −0.0020 (17) | −0.0012 (16) | −0.0068 (16) |
C2A | 0.018 (2) | 0.040 (3) | 0.021 (2) | −0.005 (2) | 0.0007 (17) | 0.002 (2) |
C3A | 0.022 (2) | 0.050 (4) | 0.034 (3) | −0.004 (2) | −0.007 (2) | 0.009 (3) |
C4A | 0.038 (3) | 0.037 (3) | 0.021 (2) | −0.004 (2) | −0.009 (2) | 0.002 (2) |
C5A | 0.041 (3) | 0.034 (3) | 0.014 (2) | 0.002 (2) | 0.006 (2) | 0.004 (2) |
C6A | 0.022 (2) | 0.026 (2) | 0.016 (2) | 0.0007 (18) | 0.0067 (17) | −0.0033 (18) |
C8A | 0.021 (2) | 0.023 (2) | 0.0141 (19) | 0.0009 (17) | 0.0058 (16) | −0.0099 (17) |
C9A | 0.027 (2) | 0.023 (2) | 0.024 (2) | 0.0072 (19) | 0.0106 (19) | −0.0064 (18) |
C10A | 0.016 (2) | 0.032 (3) | 0.037 (3) | 0.0068 (19) | 0.0107 (19) | −0.003 (2) |
C11A | 0.014 (2) | 0.033 (3) | 0.040 (3) | −0.0039 (19) | 0.0080 (19) | −0.002 (2) |
C12A | 0.021 (2) | 0.012 (2) | 0.024 (2) | 0.0018 (16) | 0.0095 (17) | −0.0055 (17) |
C13A | 0.022 (2) | 0.0118 (19) | 0.016 (2) | −0.0090 (16) | 0.0062 (16) | −0.0054 (15) |
C14A | 0.032 (2) | 0.018 (2) | 0.024 (2) | −0.0017 (18) | 0.0065 (19) | 0.0003 (16) |
C15A | 0.060 (4) | 0.016 (2) | 0.028 (3) | −0.009 (2) | 0.009 (2) | −0.003 (2) |
C16A | 0.060 (4) | 0.024 (3) | 0.038 (3) | −0.021 (3) | 0.020 (3) | −0.002 (2) |
C17A | 0.035 (3) | 0.044 (3) | 0.042 (3) | −0.021 (3) | 0.018 (2) | 0.000 (3) |
C18A | 0.024 (2) | 0.028 (3) | 0.023 (2) | −0.0040 (19) | 0.0089 (18) | 0.001 (2) |
C1B | 0.0151 (16) | 0.0154 (18) | 0.0104 (15) | −0.0007 (18) | 0.0021 (13) | 0.0005 (18) |
C2B | 0.024 (2) | 0.030 (3) | 0.025 (2) | −0.006 (2) | 0.0084 (19) | −0.015 (2) |
C3B | 0.042 (3) | 0.045 (4) | 0.035 (3) | −0.012 (3) | 0.013 (2) | −0.024 (3) |
C4B | 0.039 (3) | 0.033 (3) | 0.025 (3) | −0.014 (2) | −0.001 (2) | −0.010 (2) |
C5B | 0.020 (2) | 0.039 (3) | 0.030 (3) | −0.011 (2) | −0.0023 (19) | −0.002 (2) |
C6B | 0.0144 (19) | 0.034 (3) | 0.025 (2) | −0.0034 (18) | 0.0020 (16) | −0.006 (2) |
C7B | 0.0129 (18) | 0.020 (2) | 0.0145 (19) | −0.0056 (16) | 0.0042 (14) | 0.0032 (16) |
C8B | 0.016 (2) | 0.034 (3) | 0.020 (2) | −0.0011 (19) | 0.0019 (16) | 0.0067 (19) |
C9B | 0.023 (2) | 0.052 (4) | 0.025 (2) | −0.004 (2) | 0.0091 (19) | 0.017 (2) |
C10B | 0.016 (2) | 0.063 (4) | 0.039 (3) | −0.001 (2) | 0.014 (2) | 0.018 (3) |
C11B | 0.013 (2) | 0.050 (3) | 0.032 (3) | 0.004 (2) | 0.0058 (19) | 0.012 (2) |
C12B | 0.0143 (19) | 0.025 (2) | 0.020 (2) | 0.0000 (17) | 0.0053 (16) | 0.0061 (18) |
C13B | 0.0185 (19) | 0.0122 (19) | 0.0145 (19) | 0.0027 (16) | 0.0001 (15) | 0.0011 (15) |
C14B | 0.026 (2) | 0.023 (2) | 0.032 (3) | 0.005 (2) | 0.007 (2) | 0.000 (2) |
C15B | 0.036 (3) | 0.036 (3) | 0.057 (4) | 0.016 (3) | 0.017 (3) | 0.003 (3) |
C16B | 0.052 (4) | 0.027 (3) | 0.062 (4) | 0.025 (3) | 0.015 (3) | 0.011 (3) |
C17B | 0.054 (4) | 0.019 (2) | 0.041 (3) | 0.010 (2) | 0.009 (3) | 0.009 (2) |
C18B | 0.030 (2) | 0.020 (2) | 0.024 (2) | 0.0018 (19) | 0.006 (2) | 0.0020 (19) |
Geometric parameters (Å, º) top
Pt—N71 | 2.069 (3) | C4A—H4A | 0.9500 |
Pt—N72 | 2.071 (3) | C5A—C6A | 1.405 (6) |
Pt—P2 | 2.2685 (11) | C5A—H5A | 0.9500 |
Pt—P1 | 2.2792 (11) | C6A—H6A | 0.9500 |
P1—C7A | 1.817 (4) | C7A—C12A | 1.390 (6) |
P1—C13A | 1.827 (4) | C7A—C8A | 1.414 (6) |
P1—C1A | 1.841 (4) | C8A—C9A | 1.391 (6) |
P2—C13B | 1.834 (4) | C8A—H8A | 0.9500 |
P2—C7B | 1.834 (4) | C9A—C10A | 1.387 (7) |
P2—C1B | 1.836 (4) | C9A—H9A | 0.9500 |
N11—C21 | 1.401 (6) | C10A—C11A | 1.383 (7) |
N11—C61 | 1.412 (6) | C10A—H10A | 0.9500 |
N11—C11 | 1.476 (7) | C11A—C12A | 1.392 (6) |
C11—H11A | 0.9800 | C11A—H11D | 0.9500 |
C11—H11B | 0.9800 | C12A—H12D | 0.9500 |
C11—H11C | 0.9800 | C13A—C14A | 1.399 (6) |
C21—O21 | 1.225 (6) | C13A—C18A | 1.404 (6) |
C21—N31 | 1.377 (7) | C14A—C15A | 1.391 (7) |
N31—C41 | 1.391 (6) | C14A—H14A | 0.9500 |
N31—C31 | 1.462 (6) | C15A—C16A | 1.382 (8) |
C31—H31A | 0.9800 | C15A—H15A | 0.9500 |
C31—H31B | 0.9800 | C16A—C17A | 1.366 (9) |
C31—H31C | 0.9800 | C16A—H16A | 0.9500 |
C41—N91 | 1.349 (6) | C17A—C18A | 1.408 (7) |
C41—C51 | 1.378 (6) | C17A—H17A | 0.9500 |
C51—N71 | 1.395 (5) | C18A—H18A | 0.9500 |
C51—C61 | 1.415 (6) | C1B—C2B | 1.388 (6) |
C61—O61 | 1.233 (6) | C1B—C6B | 1.397 (6) |
N71—C81 | 1.315 (6) | C2B—C3B | 1.396 (7) |
C81—N91 | 1.341 (6) | C2B—H2B | 0.9500 |
C81—H81 | 0.9500 | C3B—C4B | 1.367 (8) |
N12—C22 | 1.402 (7) | C3B—H3B | 0.9500 |
N12—C62 | 1.412 (6) | C4B—C5B | 1.378 (8) |
N12—C12 | 1.482 (6) | C4B—H4B | 0.9500 |
C12—H12A | 0.9800 | C5B—C6B | 1.383 (7) |
C12—H12B | 0.9800 | C5B—H5B | 0.9500 |
C12—H12C | 0.9800 | C6B—H6B | 0.9500 |
C22—O22 | 1.226 (6) | C7B—C8B | 1.388 (6) |
C22—N32 | 1.374 (6) | C7B—C12B | 1.398 (6) |
N32—C42 | 1.390 (6) | C8B—C9B | 1.385 (6) |
N32—C32 | 1.460 (6) | C8B—H8B | 0.9500 |
C32—H32A | 0.9800 | C9B—C10B | 1.386 (7) |
C32—H32B | 0.9800 | C9B—H9B | 0.9500 |
C32—H32C | 0.9800 | C10B—C11B | 1.386 (7) |
C42—N92 | 1.356 (6) | C10B—H10B | 0.9500 |
C42—C52 | 1.370 (6) | C11B—C12B | 1.389 (6) |
C52—N72 | 1.390 (5) | C11B—H11E | 0.9500 |
C52—C62 | 1.423 (6) | C12B—H12E | 0.9500 |
C62—O62 | 1.231 (6) | C13B—C18B | 1.381 (6) |
N72—C82 | 1.326 (5) | C13B—C14B | 1.394 (6) |
C82—N92 | 1.375 (6) | C14B—C15B | 1.396 (7) |
C82—H82 | 0.9500 | C14B—H14B | 0.9500 |
C1A—C6A | 1.386 (6) | C15B—C16B | 1.381 (9) |
C1A—C2A | 1.397 (6) | C15B—H15B | 0.9500 |
C2A—C3A | 1.396 (7) | C16B—C17B | 1.373 (9) |
C2A—H2A | 0.9500 | C16B—H16B | 0.9500 |
C3A—C4A | 1.376 (8) | C17B—C18B | 1.391 (7) |
C3A—H3A | 0.9500 | C17B—H17B | 0.9500 |
C4A—C5A | 1.380 (8) | C18B—H18B | 0.9500 |
| | | |
N71—Pt—N72 | 87.05 (14) | C2A—C3A—H3A | 119.9 |
N71—Pt—P2 | 174.37 (10) | C3A—C4A—C5A | 119.9 (5) |
N72—Pt—P2 | 87.88 (10) | C3A—C4A—H4A | 120.1 |
N71—Pt—P1 | 87.60 (10) | C5A—C4A—H4A | 120.1 |
N72—Pt—P1 | 174.04 (11) | C4A—C5A—C6A | 120.4 (5) |
P2—Pt—P1 | 97.57 (4) | C4A—C5A—H5A | 119.8 |
C7A—P1—C13A | 107.1 (2) | C6A—C5A—H5A | 119.8 |
C7A—P1—C1A | 102.91 (19) | C1A—C6A—C5A | 120.1 (4) |
C13A—P1—C1A | 104.8 (2) | C1A—C6A—H6A | 120.0 |
C7A—P1—Pt | 111.61 (14) | C5A—C6A—H6A | 120.0 |
C13A—P1—Pt | 116.78 (14) | C12A—C7A—C8A | 119.4 (4) |
C1A—P1—Pt | 112.55 (15) | C12A—C7A—P1 | 120.1 (3) |
C13B—P2—C7B | 109.6 (2) | C8A—C7A—P1 | 120.5 (3) |
C13B—P2—C1B | 102.3 (2) | C9A—C8A—C7A | 119.1 (4) |
C7B—P2—C1B | 103.14 (18) | C9A—C8A—H8A | 120.5 |
C13B—P2—Pt | 115.97 (14) | C7A—C8A—H8A | 120.5 |
C7B—P2—Pt | 111.97 (14) | C10A—C9A—C8A | 120.7 (4) |
C1B—P2—Pt | 112.79 (14) | C10A—C9A—H9A | 119.7 |
C21—N11—C61 | 126.1 (4) | C8A—C9A—H9A | 119.7 |
C21—N11—C11 | 116.0 (4) | C11A—C10A—C9A | 120.3 (4) |
C61—N11—C11 | 117.7 (4) | C11A—C10A—H10A | 119.8 |
N11—C11—H11A | 109.5 | C9A—C10A—H10A | 119.8 |
N11—C11—H11B | 109.5 | C10A—C11A—C12A | 119.7 (4) |
H11A—C11—H11B | 109.5 | C10A—C11A—H11D | 120.1 |
N11—C11—H11C | 109.5 | C12A—C11A—H11D | 120.1 |
H11A—C11—H11C | 109.5 | C7A—C12A—C11A | 120.7 (4) |
H11B—C11—H11C | 109.5 | C7A—C12A—H12D | 119.7 |
O21—C21—N31 | 121.5 (5) | C11A—C12A—H12D | 119.7 |
O21—C21—N11 | 120.7 (5) | C14A—C13A—C18A | 118.2 (4) |
N31—C21—N11 | 117.8 (4) | C14A—C13A—P1 | 123.7 (3) |
C21—N31—C41 | 119.2 (4) | C18A—C13A—P1 | 117.9 (3) |
C21—N31—C31 | 118.5 (4) | C15A—C14A—C13A | 120.6 (5) |
C41—N31—C31 | 121.9 (4) | C15A—C14A—H14A | 119.7 |
N31—C31—H31A | 109.5 | C13A—C14A—H14A | 119.7 |
N31—C31—H31B | 109.5 | C16A—C15A—C14A | 120.6 (5) |
H31A—C31—H31B | 109.5 | C16A—C15A—H15A | 119.7 |
N31—C31—H31C | 109.5 | C14A—C15A—H15A | 119.7 |
H31A—C31—H31C | 109.5 | C17A—C16A—C15A | 119.9 (5) |
H31B—C31—H31C | 109.5 | C17A—C16A—H16A | 120.0 |
N91—C41—C51 | 111.7 (4) | C15A—C16A—H16A | 120.0 |
N91—C41—N31 | 127.0 (4) | C16A—C17A—C18A | 120.5 (5) |
C51—C41—N31 | 121.3 (4) | C16A—C17A—H17A | 119.7 |
C41—C51—N71 | 105.8 (4) | C18A—C17A—H17A | 119.7 |
C41—C51—C61 | 123.3 (4) | C13A—C18A—C17A | 120.1 (5) |
N71—C51—C61 | 130.9 (4) | C13A—C18A—H18A | 120.0 |
O61—C61—N11 | 120.1 (4) | C17A—C18A—H18A | 120.0 |
O61—C61—C51 | 127.7 (4) | C2B—C1B—C6B | 118.3 (4) |
N11—C61—C51 | 112.2 (4) | C2B—C1B—P2 | 121.6 (3) |
C81—N71—C51 | 104.0 (3) | C6B—C1B—P2 | 120.0 (3) |
C81—N71—Pt | 133.2 (3) | C1B—C2B—C3B | 120.1 (5) |
C51—N71—Pt | 122.0 (3) | C1B—C2B—H2B | 119.9 |
N71—C81—N91 | 116.5 (4) | C3B—C2B—H2B | 119.9 |
N71—C81—H81 | 121.7 | C4B—C3B—C2B | 120.6 (5) |
N91—C81—H81 | 121.7 | C4B—C3B—H3B | 119.7 |
C81—N91—C41 | 102.0 (4) | C2B—C3B—H3B | 119.7 |
C22—N12—C62 | 126.9 (4) | C3B—C4B—C5B | 120.2 (5) |
C22—N12—C12 | 116.0 (4) | C3B—C4B—H4B | 119.9 |
C62—N12—C12 | 117.1 (4) | C5B—C4B—H4B | 119.9 |
N12—C12—H12A | 109.5 | C4B—C5B—C6B | 119.7 (5) |
N12—C12—H12B | 109.5 | C4B—C5B—H5B | 120.1 |
H12A—C12—H12B | 109.5 | C6B—C5B—H5B | 120.1 |
N12—C12—H12C | 109.5 | C5B—C6B—C1B | 121.1 (4) |
H12A—C12—H12C | 109.5 | C5B—C6B—H6B | 119.5 |
H12B—C12—H12C | 109.5 | C1B—C6B—H6B | 119.5 |
O22—C22—N32 | 121.8 (5) | C8B—C7B—C12B | 119.5 (4) |
O22—C22—N12 | 120.8 (5) | C8B—C7B—P2 | 122.3 (3) |
N32—C22—N12 | 117.5 (4) | C12B—C7B—P2 | 118.0 (3) |
C22—N32—C42 | 118.9 (4) | C9B—C8B—C7B | 120.6 (4) |
C22—N32—C32 | 119.0 (4) | C9B—C8B—H8B | 119.7 |
C42—N32—C32 | 121.8 (4) | C7B—C8B—H8B | 119.7 |
N32—C32—H32A | 109.5 | C8B—C9B—C10B | 119.3 (5) |
N32—C32—H32B | 109.5 | C8B—C9B—H9B | 120.4 |
H32A—C32—H32B | 109.5 | C10B—C9B—H9B | 120.4 |
N32—C32—H32C | 109.5 | C11B—C10B—C9B | 121.1 (4) |
H32A—C32—H32C | 109.5 | C11B—C10B—H10B | 119.4 |
H32B—C32—H32C | 109.5 | C9B—C10B—H10B | 119.4 |
N92—C42—C52 | 112.1 (4) | C10B—C11B—C12B | 119.2 (4) |
N92—C42—N32 | 125.8 (4) | C10B—C11B—H11E | 120.4 |
C52—C42—N32 | 122.1 (4) | C12B—C11B—H11E | 120.4 |
C42—C52—N72 | 106.5 (4) | C11B—C12B—C7B | 120.3 (4) |
C42—C52—C62 | 123.0 (4) | C11B—C12B—H12E | 119.9 |
N72—C52—C62 | 130.5 (4) | C7B—C12B—H12E | 119.9 |
O62—C62—N12 | 120.9 (4) | C18B—C13B—C14B | 119.3 (4) |
O62—C62—C52 | 127.5 (4) | C18B—C13B—P2 | 125.0 (3) |
N12—C62—C52 | 111.5 (4) | C14B—C13B—P2 | 115.7 (3) |
C82—N72—C52 | 104.8 (3) | C13B—C14B—C15B | 120.6 (5) |
C82—N72—Pt | 130.4 (3) | C13B—C14B—H14B | 119.7 |
C52—N72—Pt | 123.6 (3) | C15B—C14B—H14B | 119.7 |
N72—C82—N92 | 114.9 (4) | C16B—C15B—C14B | 119.2 (5) |
N72—C82—H82 | 122.6 | C16B—C15B—H15B | 120.4 |
N92—C82—H82 | 122.6 | C14B—C15B—H15B | 120.4 |
C42—N92—C82 | 101.7 (4) | C17B—C16B—C15B | 120.4 (5) |
C6A—C1A—C2A | 118.9 (4) | C17B—C16B—H16B | 119.8 |
C6A—C1A—P1 | 120.1 (3) | C15B—C16B—H16B | 119.8 |
C2A—C1A—P1 | 120.8 (3) | C16B—C17B—C18B | 120.6 (5) |
C3A—C2A—C1A | 120.6 (5) | C16B—C17B—H17B | 119.7 |
C3A—C2A—H2A | 119.7 | C18B—C17B—H17B | 119.7 |
C1A—C2A—H2A | 119.7 | C13B—C18B—C17B | 119.9 (5) |
C4A—C3A—C2A | 120.1 (5) | C13B—C18B—H18B | 120.0 |
C4A—C3A—H3A | 119.9 | C17B—C18B—H18B | 120.0 |
| | | |
N71—Pt—P1—C7A | 85.86 (17) | N72—C82—N92—C42 | −0.6 (5) |
P2—Pt—P1—C7A | −96.37 (14) | C7A—P1—C1A—C6A | −24.1 (4) |
N71—Pt—P1—C13A | −150.52 (19) | C13A—P1—C1A—C6A | −135.9 (4) |
P2—Pt—P1—C13A | 27.25 (17) | Pt—P1—C1A—C6A | 96.2 (4) |
N71—Pt—P1—C1A | −29.27 (18) | C7A—P1—C1A—C2A | 160.7 (4) |
P2—Pt—P1—C1A | 148.50 (16) | C13A—P1—C1A—C2A | 48.8 (4) |
N72—Pt—P2—C13B | −142.83 (18) | Pt—P1—C1A—C2A | −79.0 (4) |
P1—Pt—P2—C13B | 34.76 (16) | C6A—C1A—C2A—C3A | −0.2 (8) |
N72—Pt—P2—C7B | 90.41 (18) | P1—C1A—C2A—C3A | 175.1 (4) |
P1—Pt—P2—C7B | −92.00 (16) | C1A—C2A—C3A—C4A | −0.3 (9) |
N72—Pt—P2—C1B | −25.40 (17) | C2A—C3A—C4A—C5A | 1.1 (9) |
P1—Pt—P2—C1B | 152.19 (14) | C3A—C4A—C5A—C6A | −1.4 (9) |
C61—N11—C21—O21 | 177.3 (5) | C2A—C1A—C6A—C5A | −0.1 (7) |
C11—N11—C21—O21 | 2.1 (8) | P1—C1A—C6A—C5A | −175.5 (4) |
C61—N11—C21—N31 | −3.9 (8) | C4A—C5A—C6A—C1A | 0.9 (8) |
C11—N11—C21—N31 | −179.1 (5) | C13A—P1—C7A—C12A | −131.8 (4) |
O21—C21—N31—C41 | 179.7 (5) | C1A—P1—C7A—C12A | 118.0 (4) |
N11—C21—N31—C41 | 0.9 (7) | Pt—P1—C7A—C12A | −2.9 (4) |
O21—C21—N31—C31 | −6.9 (8) | C13A—P1—C7A—C8A | 49.4 (4) |
N11—C21—N31—C31 | 174.3 (5) | C1A—P1—C7A—C8A | −60.7 (4) |
C21—N31—C41—N91 | 180.0 (5) | Pt—P1—C7A—C8A | 178.4 (3) |
C31—N31—C41—N91 | 6.8 (8) | C12A—C7A—C8A—C9A | 3.1 (6) |
C21—N31—C41—C51 | 1.6 (7) | P1—C7A—C8A—C9A | −178.1 (4) |
C31—N31—C41—C51 | −171.6 (5) | C7A—C8A—C9A—C10A | −1.0 (7) |
N91—C41—C51—N71 | −1.4 (5) | C8A—C9A—C10A—C11A | −2.0 (8) |
N31—C41—C51—N71 | 177.3 (4) | C9A—C10A—C11A—C12A | 2.8 (8) |
N91—C41—C51—C61 | 180.0 (4) | C8A—C7A—C12A—C11A | −2.3 (7) |
N31—C41—C51—C61 | −1.4 (7) | P1—C7A—C12A—C11A | 178.9 (4) |
C21—N11—C61—O61 | −176.4 (6) | C10A—C11A—C12A—C7A | −0.6 (7) |
C11—N11—C61—O61 | −1.3 (8) | C7A—P1—C13A—C14A | 2.6 (4) |
C21—N11—C61—C51 | 3.9 (8) | C1A—P1—C13A—C14A | 111.4 (4) |
C11—N11—C61—C51 | 179.1 (5) | Pt—P1—C13A—C14A | −123.3 (3) |
C41—C51—C61—O61 | 179.2 (6) | C7A—P1—C13A—C18A | 178.9 (3) |
N71—C51—C61—O61 | 0.9 (9) | C1A—P1—C13A—C18A | −72.2 (4) |
C41—C51—C61—N11 | −1.2 (7) | Pt—P1—C13A—C18A | 53.0 (4) |
N71—C51—C61—N11 | −179.5 (5) | C18A—C13A—C14A—C15A | 1.9 (7) |
C41—C51—N71—C81 | 1.1 (5) | P1—C13A—C14A—C15A | 178.3 (4) |
C61—C51—N71—C81 | 179.6 (5) | C13A—C14A—C15A—C16A | −0.1 (8) |
C41—C51—N71—Pt | −170.3 (3) | C14A—C15A—C16A—C17A | −1.4 (9) |
C61—C51—N71—Pt | 8.2 (7) | C15A—C16A—C17A—C18A | 1.0 (9) |
N72—Pt—N71—C81 | 97.9 (4) | C14A—C13A—C18A—C17A | −2.3 (7) |
P1—Pt—N71—C81 | −79.4 (4) | P1—C13A—C18A—C17A | −178.9 (4) |
N72—Pt—N71—C51 | −93.5 (3) | C16A—C17A—C18A—C13A | 0.9 (8) |
P1—Pt—N71—C51 | 89.1 (3) | C13B—P2—C1B—C2B | −129.3 (4) |
C51—N71—C81—N91 | −0.5 (5) | C7B—P2—C1B—C2B | −15.6 (4) |
Pt—N71—C81—N91 | 169.5 (3) | Pt—P2—C1B—C2B | 105.4 (4) |
N71—C81—N91—C41 | −0.3 (6) | C13B—P2—C1B—C6B | 54.6 (4) |
C51—C41—N91—C81 | 1.0 (5) | C7B—P2—C1B—C6B | 168.4 (4) |
N31—C41—N91—C81 | −177.6 (5) | Pt—P2—C1B—C6B | −70.6 (4) |
C62—N12—C22—O22 | 179.3 (5) | C6B—C1B—C2B—C3B | −1.3 (8) |
C12—N12—C22—O22 | −0.5 (7) | P2—C1B—C2B—C3B | −177.4 (4) |
C62—N12—C22—N32 | −1.0 (8) | C1B—C2B—C3B—C4B | 0.4 (9) |
C12—N12—C22—N32 | 179.2 (5) | C2B—C3B—C4B—C5B | 0.4 (9) |
O22—C22—N32—C42 | 177.2 (5) | C3B—C4B—C5B—C6B | −0.4 (9) |
N12—C22—N32—C42 | −2.5 (7) | C4B—C5B—C6B—C1B | −0.5 (8) |
O22—C22—N32—C32 | −9.1 (7) | C2B—C1B—C6B—C5B | 1.3 (7) |
N12—C22—N32—C32 | 171.2 (4) | P2—C1B—C6B—C5B | 177.5 (4) |
C22—N32—C42—N92 | −174.6 (5) | C13B—P2—C7B—C8B | 48.0 (5) |
C32—N32—C42—N92 | 11.9 (7) | C1B—P2—C7B—C8B | −60.3 (5) |
C22—N32—C42—C52 | 3.9 (7) | Pt—P2—C7B—C8B | 178.1 (4) |
C32—N32—C42—C52 | −169.6 (4) | C13B—P2—C7B—C12B | −137.7 (4) |
N92—C42—C52—N72 | −1.0 (5) | C1B—P2—C7B—C12B | 114.0 (4) |
N32—C42—C52—N72 | −179.7 (4) | Pt—P2—C7B—C12B | −7.6 (4) |
N92—C42—C52—C62 | 176.9 (4) | C12B—C7B—C8B—C9B | 1.1 (8) |
N32—C42—C52—C62 | −1.8 (7) | P2—C7B—C8B—C9B | 175.3 (4) |
C22—N12—C62—O62 | −178.0 (5) | C7B—C8B—C9B—C10B | 0.1 (9) |
C12—N12—C62—O62 | 1.9 (7) | C8B—C9B—C10B—C11B | −1.4 (10) |
C22—N12—C62—C52 | 2.9 (7) | C9B—C10B—C11B—C12B | 1.4 (10) |
C12—N12—C62—C52 | −177.3 (5) | C10B—C11B—C12B—C7B | −0.1 (9) |
C42—C52—C62—O62 | 179.5 (5) | C8B—C7B—C12B—C11B | −1.1 (7) |
N72—C52—C62—O62 | −3.2 (9) | P2—C7B—C12B—C11B | −175.6 (4) |
C42—C52—C62—N12 | −1.5 (7) | C7B—P2—C13B—C18B | −5.2 (5) |
N72—C52—C62—N12 | 175.9 (4) | C1B—P2—C13B—C18B | 103.7 (4) |
C42—C52—N72—C82 | 0.6 (5) | Pt—P2—C13B—C18B | −133.1 (4) |
C62—C52—N72—C82 | −177.1 (5) | C7B—P2—C13B—C14B | 175.8 (3) |
C42—C52—N72—Pt | −168.4 (3) | C1B—P2—C13B—C14B | −75.2 (4) |
C62—C52—N72—Pt | 13.9 (7) | Pt—P2—C13B—C14B | 47.9 (4) |
N71—Pt—N72—C82 | 102.3 (4) | C18B—C13B—C14B—C15B | −1.9 (7) |
P2—Pt—N72—C82 | −75.2 (4) | P2—C13B—C14B—C15B | 177.1 (4) |
N71—Pt—N72—C52 | −91.8 (3) | C13B—C14B—C15B—C16B | 0.5 (9) |
P2—Pt—N72—C52 | 90.7 (3) | C14B—C15B—C16B—C17B | 1.3 (10) |
C52—N72—C82—N92 | 0.0 (5) | C15B—C16B—C17B—C18B | −1.7 (10) |
Pt—N72—C82—N92 | 167.9 (3) | C14B—C13B—C18B—C17B | 1.6 (7) |
C52—C42—N92—C82 | 1.0 (5) | P2—C13B—C18B—C17B | −177.4 (4) |
N32—C42—N92—C82 | 179.6 (4) | C16B—C17B—C18B—C13B | 0.2 (9) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C4B—H4B···O21i | 0.95 | 2.42 | 3.065 (6) | 125 |
C10A—H10A···O22ii | 0.95 | 2.51 | 3.184 (6) | 128 |
Symmetry codes: (i) x+1, −y+1/2, z+1/2; (ii) −x+2, y−1/2, −z+3/2. |
(II)
cis-chloro(1,2,3,6-tetrahydro-3,7-dimethylpurine-2,6-dionato-
κN1)bis (triphenylphosphine-
κP)platinum(II) ethanol
hemisolvate
top
Crystal data top
[PtCl(C7H7N4O2)(C18H15P)2]·0.5C2H6O | Z = 4 |
Mr = 957.28 | F(000) = 1908 |
Triclinic, P1 | Dx = 1.589 Mg m−3 |
a = 11.4777 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 19.3276 (13) Å | Cell parameters from 8000 reflections |
c = 20.5946 (17) Å | θ = 2.7–29.3° |
α = 62.565 (8)° | µ = 3.70 mm−1 |
β = 81.354 (10)° | T = 183 K |
γ = 89.019 (9)° | Plate, colourless |
V = 4001.7 (5) Å3 | 0.36 × 0.18 × 0.06 mm |
Data collection top
Stoe IPDS diffractometer | 19993 independent reflections |
Radiation source: fine-focus sealed tube | 8805 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.096 |
ϕ oscillation scan | θmax = 29.3°, θmin = 2.7° |
Absorption correction: numerical (Coppens et al., 1965) | h = −15→15 |
Tmin = 0.350, Tmax = 0.809 | k = −23→25 |
43394 measured reflections | l = 0→28 |
Refinement top
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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.69 | w = 1/[σ2(Fo2) + (0.03P)2] where P = (Fo2 + 2Fc2)/3 |
19993 reflections | (Δ/σ)max = 0.002 |
839 parameters | Δρmax = 1.40 e Å−3 |
59 restraints | Δρmin = −2.62 e Å−3 |
Crystal data top
[PtCl(C7H7N4O2)(C18H15P)2]·0.5C2H6O | γ = 89.019 (9)° |
Mr = 957.28 | V = 4001.7 (5) Å3 |
Triclinic, P1 | Z = 4 |
a = 11.4777 (9) Å | Mo Kα radiation |
b = 19.3276 (13) Å | µ = 3.70 mm−1 |
c = 20.5946 (17) Å | T = 183 K |
α = 62.565 (8)° | 0.36 × 0.18 × 0.06 mm |
β = 81.354 (10)° | |
Data collection top
Stoe IPDS diffractometer | 19993 independent reflections |
Absorption correction: numerical (Coppens et al., 1965) | 8805 reflections with I > 2σ(I) |
Tmin = 0.350, Tmax = 0.809 | Rint = 0.096 |
43394 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.042 | 59 restraints |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.69 | Δρmax = 1.40 e Å−3 |
19993 reflections | Δρmin = −2.62 e Å−3 |
839 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Pt1 | 0.43721 (2) | 0.095320 (18) | 0.720400 (15) | 0.02690 (8) | |
Cl1 | 0.44451 (18) | 0.14168 (12) | 0.80662 (10) | 0.0444 (5) | |
P1 | 0.44137 (14) | 0.05944 (11) | 0.63108 (10) | 0.0262 (4) | |
C1A | 0.4627 (4) | 0.1412 (2) | 0.53581 (19) | 0.0288 (16) | |
C2A | 0.5698 (3) | 0.1580 (3) | 0.4884 (2) | 0.0331 (18) | |
H2A | 0.6336 | 0.1254 | 0.5037 | 0.040* | |
C3A | 0.5836 (3) | 0.2224 (3) | 0.4185 (2) | 0.042 (2) | |
H3A | 0.6568 | 0.2338 | 0.3861 | 0.051* | |
C4A | 0.4902 (4) | 0.2700 (3) | 0.3961 (2) | 0.041 (2) | |
H4A | 0.4997 | 0.3140 | 0.3483 | 0.049* | |
C5A | 0.3831 (3) | 0.2533 (3) | 0.4435 (2) | 0.040 (2) | |
H5A | 0.3193 | 0.2858 | 0.4282 | 0.048* | |
C6A | 0.3693 (3) | 0.1889 (3) | 0.5134 (2) | 0.0346 (18) | |
H6A | 0.2961 | 0.1774 | 0.5458 | 0.041* | |
C1B | 0.5672 (3) | 0.0002 (3) | 0.6315 (3) | 0.0260 (16) | |
C2B | 0.6742 (4) | 0.0304 (2) | 0.6344 (3) | 0.0317 (17) | |
H2B | 0.6771 | 0.0770 | 0.6390 | 0.038* | |
C3B | 0.7769 (3) | −0.0077 (3) | 0.6307 (3) | 0.038 (2) | |
H3B | 0.8500 | 0.0130 | 0.6327 | 0.046* | |
C4B | 0.7727 (3) | −0.0759 (3) | 0.6241 (3) | 0.044 (2) | |
H4B | 0.8429 | −0.1019 | 0.6215 | 0.053* | |
C5B | 0.6657 (4) | −0.1061 (2) | 0.6211 (3) | 0.042 (2) | |
H5B | 0.6628 | −0.1528 | 0.6166 | 0.050* | |
C6B | 0.5629 (3) | −0.0681 (3) | 0.6249 (3) | 0.0310 (18) | |
H6B | 0.4898 | −0.0888 | 0.6228 | 0.037* | |
C1C | 0.3059 (3) | 0.0116 (3) | 0.6315 (3) | 0.0324 (18) | |
C2C | 0.3011 (3) | −0.0197 (3) | 0.5832 (2) | 0.039 (2) | |
H2C | 0.3691 | −0.0159 | 0.5489 | 0.047* | |
C3C | 0.1967 (5) | −0.0564 (4) | 0.5849 (3) | 0.060 (3) | |
H3C | 0.1934 | −0.0777 | 0.5519 | 0.072* | |
C4C | 0.0971 (4) | −0.0618 (4) | 0.6351 (4) | 0.079 (4) | |
H4C | 0.0258 | −0.0869 | 0.6363 | 0.095* | |
C5C | 0.1019 (3) | −0.0305 (4) | 0.6834 (3) | 0.062 (3) | |
H5C | 0.0339 | −0.0342 | 0.7177 | 0.075* | |
C6C | 0.2063 (4) | 0.0062 (3) | 0.6816 (3) | 0.043 (2) | |
H6C | 0.2096 | 0.0276 | 0.7147 | 0.052* | |
P2 | 0.43415 (15) | −0.02514 (11) | 0.81853 (10) | 0.0287 (4) | |
C1D | 0.5521 (3) | −0.0300 (3) | 0.8711 (2) | 0.0313 (18) | |
C2D | 0.6652 (4) | −0.0037 (4) | 0.8316 (2) | 0.054 (3) | |
H2D | 0.6790 | 0.0158 | 0.7793 | 0.064* | |
C3D | 0.7582 (3) | −0.0059 (4) | 0.8685 (3) | 0.073 (4) | |
H3D | 0.8356 | 0.0121 | 0.8415 | 0.088* | |
C4D | 0.7380 (4) | −0.0343 (4) | 0.9450 (3) | 0.067 (3) | |
H4D | 0.8016 | −0.0358 | 0.9702 | 0.081* | |
C5D | 0.6249 (5) | −0.0606 (4) | 0.9845 (2) | 0.066 (3) | |
H5D | 0.6111 | −0.0801 | 1.0368 | 0.080* | |
C6D | 0.5319 (4) | −0.0585 (4) | 0.9476 (2) | 0.051 (2) | |
H6D | 0.4545 | −0.0765 | 0.9746 | 0.061* | |
C1E | 0.4473 (4) | −0.1147 (2) | 0.8083 (3) | 0.0307 (18) | |
C2E | 0.5514 (3) | −0.1534 (3) | 0.8139 (3) | 0.0368 (19) | |
H2E | 0.6184 | −0.1341 | 0.8240 | 0.044* | |
C3E | 0.5576 (4) | −0.2203 (3) | 0.8047 (3) | 0.049 (2) | |
H3E | 0.6288 | −0.2467 | 0.8085 | 0.059* | |
C4E | 0.4596 (5) | −0.2486 (3) | 0.7900 (3) | 0.047 (2) | |
H4E | 0.4638 | −0.2943 | 0.7837 | 0.056* | |
C5E | 0.3555 (4) | −0.2099 (3) | 0.7844 (3) | 0.043 (2) | |
H5E | 0.2885 | −0.2292 | 0.7743 | 0.052* | |
C6E | 0.3493 (3) | −0.1430 (3) | 0.7936 (3) | 0.0349 (18) | |
H6E | 0.2781 | −0.1166 | 0.7898 | 0.042* | |
C1F | 0.2915 (3) | −0.0454 (3) | 0.8801 (2) | 0.0351 (18) | |
C2F | 0.2644 (4) | −0.1186 (3) | 0.9409 (3) | 0.051 (2) | |
H2F | 0.3202 | −0.1577 | 0.9513 | 0.061* | |
C3F | 0.1555 (5) | −0.1346 (3) | 0.9866 (3) | 0.067 (3) | |
H3F | 0.1370 | −0.1846 | 1.0282 | 0.080* | |
C4F | 0.0739 (4) | −0.0774 (4) | 0.9714 (3) | 0.059 (3) | |
H4F | −0.0005 | −0.0883 | 1.0026 | 0.070* | |
C5F | 0.1010 (4) | −0.0042 (3) | 0.9105 (3) | 0.051 (2) | |
H5F | 0.0452 | 0.0348 | 0.9001 | 0.062* | |
C6F | 0.2098 (4) | 0.0118 (2) | 0.8649 (3) | 0.040 (2) | |
H6F | 0.2284 | 0.0618 | 0.8233 | 0.048* | |
N11 | 0.4249 (4) | 0.2108 (3) | 0.6430 (3) | 0.0350 (16) | |
C21 | 0.3085 (6) | 0.2345 (4) | 0.6392 (4) | 0.038 (2) | |
O21 | 0.2238 (4) | 0.1882 (3) | 0.6784 (3) | 0.0536 (18) | |
N31 | 0.2939 (5) | 0.3108 (4) | 0.5869 (4) | 0.055 (2) | |
C31 | 0.1709 (8) | 0.3384 (6) | 0.5774 (6) | 0.098 (4) | |
H31A | 0.1722 | 0.3949 | 0.5605 | 0.147* | |
H31B | 0.1179 | 0.3115 | 0.6249 | 0.147* | |
H31C | 0.1428 | 0.3269 | 0.5406 | 0.147* | |
C41 | 0.3884 (6) | 0.3558 (4) | 0.5408 (4) | 0.054 (3) | |
C51 | 0.5050 (6) | 0.3340 (4) | 0.5460 (4) | 0.040 (2) | |
C61 | 0.5244 (6) | 0.2558 (4) | 0.5994 (4) | 0.0343 (18) | |
O61 | 0.6241 (4) | 0.2290 (3) | 0.6060 (3) | 0.0428 (14) | |
N71 | 0.5734 (6) | 0.3937 (4) | 0.4901 (4) | 0.065 (2) | |
C71 | 0.6995 (8) | 0.3986 (7) | 0.4715 (6) | 0.090 (4) | |
H71A | 0.7338 | 0.3677 | 0.5164 | 0.135* | |
H71B | 0.7291 | 0.4533 | 0.4493 | 0.135* | |
H71C | 0.7218 | 0.3783 | 0.4359 | 0.135* | |
C81 | 0.4969 (9) | 0.4510 (5) | 0.4546 (6) | 0.105 (5) | |
H81 | 0.5231 | 0.5000 | 0.4133 | 0.126* | |
N91 | 0.3817 (8) | 0.4300 (4) | 0.4847 (5) | 0.079 (3) | |
Pt2 | 0.89161 (2) | 0.459200 (18) | 0.216950 (17) | 0.03039 (9) | |
Cl2 | 0.74624 (15) | 0.36053 (12) | 0.24694 (12) | 0.0433 (5) | |
P3 | 1.01274 (15) | 0.56318 (11) | 0.18796 (11) | 0.0305 (4) | |
C1G | 0.9399 (4) | 0.6561 (2) | 0.1577 (2) | 0.0282 (16) | |
C2G | 0.8974 (5) | 0.6822 (3) | 0.2090 (2) | 0.043 (2) | |
H2G | 0.9118 | 0.6543 | 0.2586 | 0.051* | |
C3G | 0.8339 (5) | 0.7490 (3) | 0.1876 (3) | 0.053 (2) | |
H3G | 0.8049 | 0.7668 | 0.2227 | 0.063* | |
C4G | 0.8129 (4) | 0.7897 (2) | 0.1150 (3) | 0.045 (2) | |
H4G | 0.7695 | 0.8354 | 0.1004 | 0.054* | |
C5G | 0.8554 (4) | 0.7637 (3) | 0.0637 (2) | 0.043 (2) | |
H5G | 0.8410 | 0.7915 | 0.0141 | 0.051* | |
C6G | 0.9189 (4) | 0.6969 (3) | 0.0851 (2) | 0.0360 (19) | |
H6G | 0.9479 | 0.6791 | 0.0501 | 0.043* | |
C1H | 1.0669 (5) | 0.5524 (4) | 0.2710 (3) | 0.043 (2) | |
C2H | 1.1650 (6) | 0.5928 (5) | 0.2701 (3) | 0.117 (6) | |
H2H | 1.2117 | 0.6279 | 0.2245 | 0.140* | |
C3H | 1.1945 (7) | 0.5814 (6) | 0.3376 (5) | 0.177 (10) | |
H3H | 1.2609 | 0.6103 | 0.3372 | 0.212* | |
C4H | 1.1326 (8) | 0.5312 (6) | 0.4023 (4) | 0.122 (6) | |
H4H | 1.1572 | 0.5228 | 0.4473 | 0.146* | |
C5H | 1.0352 (7) | 0.4926 (5) | 0.4040 (3) | 0.088 (4) | |
H5H | 0.9890 | 0.4582 | 0.4500 | 0.106* | |
C6H | 1.0023 (5) | 0.5030 (4) | 0.3377 (3) | 0.054 (3) | |
H6H | 0.9336 | 0.4753 | 0.3391 | 0.065* | |
C1I | 1.1296 (4) | 0.5849 (3) | 0.1096 (2) | 0.0332 (19) | |
C2I | 1.2259 (5) | 0.6371 (4) | 0.0900 (3) | 0.073 (3) | |
H2I | 1.2359 | 0.6616 | 0.1198 | 0.088* | |
C3I | 1.3076 (4) | 0.6535 (4) | 0.0269 (4) | 0.080 (4) | |
H3I | 1.3734 | 0.6892 | 0.0136 | 0.095* | |
C4I | 1.2929 (5) | 0.6177 (4) | −0.0166 (3) | 0.069 (3) | |
H4I | 1.3487 | 0.6289 | −0.0597 | 0.083* | |
C5I | 1.1966 (5) | 0.5655 (4) | 0.0029 (3) | 0.055 (3) | |
H5I | 1.1865 | 0.5410 | −0.0268 | 0.066* | |
C6I | 1.1149 (4) | 0.5491 (3) | 0.0660 (3) | 0.042 (2) | |
H6I | 1.0491 | 0.5135 | 0.0794 | 0.051* | |
P4 | 1.02964 (15) | 0.36739 (11) | 0.25129 (10) | 0.0310 (5) | |
C1K | 1.1883 (3) | 0.3990 (3) | 0.2335 (3) | 0.0362 (19) | |
C2K | 1.2585 (4) | 0.4085 (3) | 0.1684 (3) | 0.043 (2) | |
H2K | 1.2257 | 0.3977 | 0.1341 | 0.051* | |
C3K | 1.3767 (4) | 0.4338 (3) | 0.1536 (3) | 0.057 (3) | |
H3K | 1.4247 | 0.4403 | 0.1091 | 0.068* | |
C4K | 1.4246 (3) | 0.4495 (3) | 0.2038 (4) | 0.065 (3) | |
H4K | 1.5054 | 0.4668 | 0.1936 | 0.078* | |
C5K | 1.3544 (4) | 0.4400 (3) | 0.2688 (3) | 0.061 (3) | |
H5K | 1.3871 | 0.4508 | 0.3032 | 0.073* | |
C6K | 1.2362 (4) | 0.4148 (3) | 0.2837 (2) | 0.047 (2) | |
H6K | 1.1882 | 0.4083 | 0.3282 | 0.056* | |
C1L | 1.0048 (4) | 0.2987 (3) | 0.35143 (19) | 0.0297 (17) | |
C2L | 1.0918 (3) | 0.2493 (3) | 0.3838 (2) | 0.038 (2) | |
H2L | 1.1656 | 0.2517 | 0.3546 | 0.046* | |
C3L | 1.0709 (4) | 0.1964 (3) | 0.4588 (2) | 0.047 (2) | |
H3L | 1.1304 | 0.1627 | 0.4809 | 0.056* | |
C4L | 0.9630 (4) | 0.1929 (3) | 0.50151 (19) | 0.052 (2) | |
H4L | 0.9487 | 0.1567 | 0.5528 | 0.062* | |
C5L | 0.8760 (4) | 0.2422 (3) | 0.4692 (2) | 0.050 (2) | |
H5L | 0.8023 | 0.2398 | 0.4984 | 0.060* | |
C6L | 0.8969 (3) | 0.2951 (3) | 0.3941 (2) | 0.040 (2) | |
H6L | 0.8375 | 0.3288 | 0.3721 | 0.048* | |
C1M | 1.0313 (4) | 0.3070 (3) | 0.2035 (2) | 0.0320 (18) | |
C2M | 1.0978 (4) | 0.2415 (3) | 0.2253 (2) | 0.043 (2) | |
H2M | 1.1431 | 0.2289 | 0.2639 | 0.052* | |
C3M | 1.0979 (5) | 0.1944 (3) | 0.1907 (3) | 0.051 (2) | |
H3M | 1.1434 | 0.1497 | 0.2057 | 0.061* | |
C4M | 1.0316 (5) | 0.2129 (3) | 0.1343 (3) | 0.052 (2) | |
H4M | 1.0317 | 0.1807 | 0.1107 | 0.063* | |
C5M | 0.9651 (4) | 0.2784 (3) | 0.1125 (3) | 0.054 (3) | |
H5M | 0.9198 | 0.2910 | 0.0739 | 0.064* | |
C6M | 0.9650 (4) | 0.3254 (3) | 0.1471 (3) | 0.039 (2) | |
H6M | 0.9196 | 0.3702 | 0.1322 | 0.047* | |
N12 | 0.7550 (5) | 0.5351 (3) | 0.1839 (3) | 0.0402 (17) | |
C22 | 0.7491 (7) | 0.5652 (5) | 0.1083 (4) | 0.049 (2) | |
O22 | 0.8141 (5) | 0.5471 (4) | 0.0672 (3) | 0.0575 (18) | |
N32 | 0.6630 (6) | 0.6189 (5) | 0.0795 (4) | 0.073 (3) | |
C32 | 0.6569 (9) | 0.6588 (8) | −0.0032 (6) | 0.126 (6) | |
H32A | 0.6134 | 0.6241 | −0.0151 | 0.189* | |
H32B | 0.7371 | 0.6707 | −0.0314 | 0.189* | |
H32C | 0.6164 | 0.7074 | −0.0162 | 0.189* | |
C42 | 0.6012 (7) | 0.6435 (5) | 0.1242 (5) | 0.067 (3) | |
C52 | 0.6068 (6) | 0.6133 (5) | 0.1996 (5) | 0.056 (3) | |
C62 | 0.6914 (6) | 0.5559 (4) | 0.2330 (4) | 0.041 (2) | |
O62 | 0.7085 (5) | 0.5269 (4) | 0.2983 (3) | 0.0555 (17) | |
N72 | 0.5364 (7) | 0.6570 (5) | 0.2221 (5) | 0.082 (3) | |
C72 | 0.5270 (10) | 0.6501 (7) | 0.2942 (5) | 0.085 (4) | |
H72A | 0.4638 | 0.6109 | 0.3274 | 0.128* | |
H72B | 0.5088 | 0.7006 | 0.2925 | 0.128* | |
H72C | 0.6019 | 0.6341 | 0.3127 | 0.128* | |
C82 | 0.4884 (9) | 0.7080 (6) | 0.1599 (6) | 0.083 (4) | |
H82 | 0.4323 | 0.7440 | 0.1619 | 0.099* | |
N92 | 0.5251 (7) | 0.7037 (5) | 0.0977 (5) | 0.076 (3) | |
C45 | 0.834 (4) | 0.198 (3) | 0.783 (2) | 0.153 (10)* | 0.406 (10) |
H45A | 0.7982 | 0.2245 | 0.8105 | 0.229* | 0.406 (10) |
H45B | 0.9081 | 0.2263 | 0.7517 | 0.229* | 0.406 (10) |
H45C | 0.8504 | 0.1445 | 0.8172 | 0.229* | 0.406 (10) |
C43 | 0.750 (3) | 0.195 (4) | 0.734 (3) | 0.207 (14)* | 0.406 (10) |
H43A | 0.6787 | 0.1619 | 0.7653 | 0.248* | 0.406 (10) |
H43B | 0.7259 | 0.2481 | 0.7035 | 0.248* | 0.406 (10) |
O5 | 0.804 (2) | 0.1634 (17) | 0.6846 (14) | 0.120 (5)* | 0.406 (10) |
H5 | 0.777 (19) | 0.165 (18) | 0.634 (12) | 0.179* | 0.406 (10) |
C49 | −0.186 (2) | 0.2073 (19) | 0.6937 (18) | 0.153 (10)* | 0.594 (10) |
H49A | −0.1681 | 0.2570 | 0.6484 | 0.229* | 0.594 (10) |
H49B | −0.2322 | 0.2163 | 0.7329 | 0.229* | 0.594 (10) |
H49C | −0.2314 | 0.1715 | 0.6840 | 0.229* | 0.594 (10) |
C47 | −0.072 (3) | 0.1717 (19) | 0.718 (2) | 0.207 (14)* | 0.594 (10) |
H47A | −0.0109 | 0.2151 | 0.6978 | 0.248* | 0.594 (10) |
H47B | −0.0833 | 0.1498 | 0.7728 | 0.248* | 0.594 (10) |
O6 | −0.0238 (13) | 0.1127 (10) | 0.7008 (9) | 0.120 (5)* | 0.594 (10) |
H6 | 0.068 (2) | 0.101 (8) | 0.683 (12) | 0.179* | 0.594 (10) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pt1 | 0.02653 (16) | 0.0303 (2) | 0.02201 (16) | 0.00796 (13) | −0.00739 (12) | −0.00972 (14) |
Cl1 | 0.0603 (12) | 0.0396 (12) | 0.0343 (11) | 0.0090 (9) | −0.0128 (9) | −0.0167 (9) |
P1 | 0.0204 (8) | 0.0336 (11) | 0.0228 (9) | 0.0054 (7) | −0.0063 (7) | −0.0107 (8) |
C1A | 0.025 (3) | 0.036 (4) | 0.023 (4) | 0.000 (3) | −0.007 (3) | −0.011 (3) |
C2A | 0.026 (3) | 0.036 (4) | 0.027 (4) | 0.004 (3) | −0.006 (3) | −0.005 (3) |
C3A | 0.036 (4) | 0.045 (5) | 0.039 (5) | 0.000 (4) | −0.001 (3) | −0.014 (4) |
C4A | 0.046 (5) | 0.040 (5) | 0.027 (4) | 0.002 (4) | −0.013 (3) | −0.005 (4) |
C5A | 0.037 (4) | 0.047 (5) | 0.029 (4) | 0.010 (4) | −0.013 (3) | −0.010 (4) |
C6A | 0.027 (4) | 0.046 (5) | 0.026 (4) | 0.004 (3) | −0.007 (3) | −0.012 (3) |
C1B | 0.022 (3) | 0.032 (4) | 0.022 (3) | 0.002 (3) | 0.001 (3) | −0.012 (3) |
C2B | 0.029 (4) | 0.029 (4) | 0.043 (4) | 0.008 (3) | −0.013 (3) | −0.020 (4) |
C3B | 0.020 (3) | 0.043 (5) | 0.046 (5) | 0.005 (3) | −0.013 (3) | −0.014 (4) |
C4B | 0.030 (4) | 0.040 (5) | 0.056 (5) | 0.016 (3) | −0.012 (4) | −0.017 (4) |
C5B | 0.035 (4) | 0.038 (5) | 0.052 (5) | 0.006 (3) | −0.004 (4) | −0.021 (4) |
C6B | 0.027 (4) | 0.035 (5) | 0.032 (4) | 0.007 (3) | −0.011 (3) | −0.014 (3) |
C1C | 0.026 (4) | 0.040 (5) | 0.028 (4) | 0.006 (3) | −0.009 (3) | −0.012 (4) |
C2C | 0.028 (4) | 0.053 (6) | 0.036 (4) | 0.001 (3) | −0.014 (3) | −0.018 (4) |
C3C | 0.037 (5) | 0.085 (8) | 0.073 (7) | 0.002 (5) | −0.026 (5) | −0.044 (6) |
C4C | 0.019 (4) | 0.120 (10) | 0.089 (8) | −0.014 (5) | −0.012 (5) | −0.039 (8) |
C5C | 0.024 (4) | 0.092 (8) | 0.059 (6) | 0.000 (4) | 0.000 (4) | −0.027 (6) |
C6C | 0.024 (4) | 0.053 (6) | 0.038 (5) | −0.001 (3) | −0.003 (3) | −0.010 (4) |
P2 | 0.0261 (9) | 0.0329 (11) | 0.0230 (9) | 0.0036 (8) | −0.0059 (7) | −0.0089 (8) |
C1D | 0.036 (4) | 0.026 (4) | 0.026 (4) | 0.006 (3) | −0.012 (3) | −0.005 (3) |
C2D | 0.039 (5) | 0.067 (7) | 0.043 (5) | −0.012 (4) | −0.021 (4) | −0.011 (5) |
C3D | 0.052 (6) | 0.069 (7) | 0.064 (7) | −0.018 (5) | −0.038 (5) | 0.009 (5) |
C4D | 0.066 (6) | 0.064 (7) | 0.062 (6) | 0.008 (5) | −0.045 (5) | −0.010 (5) |
C5D | 0.063 (6) | 0.102 (9) | 0.031 (5) | 0.026 (6) | −0.023 (4) | −0.024 (5) |
C6D | 0.049 (5) | 0.076 (7) | 0.024 (4) | 0.015 (4) | −0.011 (4) | −0.019 (4) |
C1E | 0.023 (3) | 0.037 (5) | 0.024 (4) | 0.001 (3) | 0.000 (3) | −0.009 (3) |
C2E | 0.032 (4) | 0.042 (5) | 0.040 (4) | 0.011 (3) | −0.010 (3) | −0.020 (4) |
C3E | 0.044 (5) | 0.045 (6) | 0.055 (6) | 0.006 (4) | −0.001 (4) | −0.023 (5) |
C4E | 0.049 (5) | 0.050 (6) | 0.039 (5) | 0.010 (4) | −0.003 (4) | −0.019 (4) |
C5E | 0.042 (4) | 0.046 (5) | 0.039 (5) | −0.005 (4) | −0.008 (4) | −0.016 (4) |
C6E | 0.033 (4) | 0.034 (5) | 0.038 (4) | 0.002 (3) | −0.008 (3) | −0.016 (4) |
C1F | 0.028 (4) | 0.042 (5) | 0.029 (4) | −0.002 (3) | 0.002 (3) | −0.013 (4) |
C2F | 0.046 (5) | 0.048 (6) | 0.038 (5) | −0.001 (4) | 0.012 (4) | −0.010 (4) |
C3F | 0.058 (6) | 0.066 (7) | 0.044 (5) | −0.011 (5) | 0.017 (4) | −0.007 (5) |
C4F | 0.038 (5) | 0.080 (8) | 0.067 (7) | −0.014 (5) | 0.019 (4) | −0.050 (6) |
C5F | 0.033 (4) | 0.061 (6) | 0.057 (6) | 0.002 (4) | 0.006 (4) | −0.028 (5) |
C6F | 0.029 (4) | 0.054 (6) | 0.037 (5) | 0.009 (4) | −0.003 (3) | −0.021 (4) |
N11 | 0.037 (3) | 0.030 (4) | 0.024 (3) | 0.013 (3) | −0.002 (3) | −0.001 (3) |
C21 | 0.046 (5) | 0.035 (5) | 0.028 (4) | 0.026 (4) | −0.014 (4) | −0.009 (4) |
O21 | 0.039 (3) | 0.068 (4) | 0.035 (3) | 0.029 (3) | −0.007 (3) | −0.009 (3) |
N31 | 0.058 (5) | 0.050 (5) | 0.048 (4) | 0.029 (4) | −0.019 (4) | −0.012 (4) |
C31 | 0.087 (8) | 0.076 (8) | 0.105 (9) | 0.057 (7) | −0.028 (7) | −0.019 (7) |
C41 | 0.071 (6) | 0.036 (5) | 0.047 (5) | 0.016 (5) | −0.016 (5) | −0.011 (4) |
C51 | 0.062 (5) | 0.026 (4) | 0.024 (4) | 0.007 (4) | −0.005 (4) | −0.004 (3) |
C61 | 0.050 (5) | 0.019 (4) | 0.029 (4) | 0.008 (3) | −0.008 (3) | −0.006 (3) |
O61 | 0.035 (3) | 0.039 (3) | 0.046 (3) | 0.004 (2) | −0.009 (2) | −0.012 (3) |
N71 | 0.084 (6) | 0.038 (5) | 0.055 (5) | −0.003 (4) | −0.009 (4) | −0.007 (4) |
C71 | 0.091 (9) | 0.067 (8) | 0.086 (9) | −0.003 (6) | −0.009 (7) | −0.015 (7) |
C81 | 0.158 (13) | 0.041 (7) | 0.088 (9) | 0.024 (8) | −0.058 (9) | 0.004 (6) |
N91 | 0.094 (7) | 0.045 (5) | 0.071 (6) | 0.018 (5) | −0.022 (5) | −0.001 (5) |
Pt2 | 0.02214 (16) | 0.02350 (19) | 0.0401 (2) | 0.00313 (13) | −0.00728 (14) | −0.00960 (16) |
Cl2 | 0.0291 (9) | 0.0362 (11) | 0.0593 (13) | −0.0021 (8) | −0.0049 (8) | −0.0182 (10) |
P3 | 0.0261 (9) | 0.0253 (11) | 0.0360 (11) | 0.0018 (7) | −0.0084 (8) | −0.0098 (9) |
C1G | 0.024 (3) | 0.025 (4) | 0.033 (4) | −0.003 (3) | −0.002 (3) | −0.011 (3) |
C2G | 0.054 (5) | 0.039 (5) | 0.031 (4) | 0.005 (4) | −0.004 (4) | −0.014 (4) |
C3G | 0.068 (6) | 0.040 (5) | 0.051 (6) | 0.006 (4) | −0.002 (4) | −0.024 (4) |
C4G | 0.038 (4) | 0.026 (4) | 0.055 (5) | 0.006 (3) | 0.007 (4) | −0.010 (4) |
C5G | 0.040 (4) | 0.041 (5) | 0.036 (4) | 0.011 (4) | −0.007 (3) | −0.009 (4) |
C6G | 0.031 (4) | 0.033 (5) | 0.033 (4) | 0.004 (3) | 0.001 (3) | −0.007 (3) |
C1H | 0.040 (4) | 0.039 (5) | 0.041 (5) | −0.002 (4) | −0.017 (4) | −0.008 (4) |
C2H | 0.123 (10) | 0.135 (13) | 0.061 (7) | −0.080 (9) | −0.043 (7) | −0.009 (8) |
C3H | 0.145 (14) | 0.25 (2) | 0.078 (10) | −0.108 (14) | −0.058 (10) | −0.016 (12) |
C4H | 0.124 (12) | 0.174 (17) | 0.072 (9) | −0.008 (11) | −0.048 (9) | −0.051 (10) |
C5H | 0.091 (8) | 0.115 (11) | 0.052 (7) | 0.004 (7) | −0.032 (6) | −0.027 (7) |
C6H | 0.051 (5) | 0.067 (7) | 0.038 (5) | −0.001 (5) | −0.010 (4) | −0.019 (5) |
C1I | 0.028 (4) | 0.027 (4) | 0.042 (5) | 0.005 (3) | −0.004 (3) | −0.015 (4) |
C2I | 0.038 (5) | 0.095 (9) | 0.078 (7) | −0.026 (5) | 0.020 (5) | −0.041 (7) |
C3I | 0.039 (5) | 0.105 (10) | 0.089 (8) | −0.021 (5) | 0.017 (5) | −0.047 (8) |
C4I | 0.042 (5) | 0.090 (9) | 0.051 (6) | 0.027 (5) | 0.001 (5) | −0.017 (6) |
C5I | 0.058 (6) | 0.060 (7) | 0.044 (5) | 0.022 (5) | −0.017 (4) | −0.021 (5) |
C6I | 0.044 (5) | 0.037 (5) | 0.038 (5) | 0.000 (4) | −0.009 (4) | −0.010 (4) |
P4 | 0.0248 (9) | 0.0257 (11) | 0.0340 (11) | 0.0039 (7) | −0.0060 (8) | −0.0065 (9) |
C1K | 0.024 (3) | 0.022 (4) | 0.047 (5) | 0.006 (3) | −0.007 (3) | −0.002 (3) |
C2K | 0.029 (4) | 0.031 (5) | 0.057 (5) | 0.003 (3) | −0.003 (4) | −0.012 (4) |
C3K | 0.037 (5) | 0.031 (5) | 0.078 (7) | 0.002 (4) | 0.004 (4) | −0.008 (5) |
C4K | 0.031 (5) | 0.035 (5) | 0.104 (9) | 0.003 (4) | −0.005 (5) | −0.013 (6) |
C5K | 0.035 (5) | 0.047 (6) | 0.085 (7) | 0.001 (4) | −0.025 (5) | −0.013 (5) |
C6K | 0.035 (4) | 0.042 (5) | 0.047 (5) | 0.002 (3) | −0.018 (4) | −0.003 (4) |
C1L | 0.030 (4) | 0.022 (4) | 0.032 (4) | 0.001 (3) | −0.003 (3) | −0.009 (3) |
C2L | 0.034 (4) | 0.038 (5) | 0.030 (4) | 0.008 (3) | −0.008 (3) | −0.004 (4) |
C3L | 0.039 (4) | 0.044 (5) | 0.040 (5) | 0.010 (4) | −0.013 (4) | −0.004 (4) |
C4L | 0.057 (5) | 0.051 (6) | 0.027 (4) | −0.004 (4) | −0.006 (4) | −0.002 (4) |
C5L | 0.037 (4) | 0.056 (6) | 0.043 (5) | 0.001 (4) | 0.000 (4) | −0.014 (4) |
C6L | 0.038 (4) | 0.042 (5) | 0.035 (4) | −0.002 (3) | −0.004 (3) | −0.013 (4) |
C1M | 0.030 (4) | 0.027 (4) | 0.026 (4) | 0.005 (3) | 0.000 (3) | −0.003 (3) |
C2M | 0.041 (4) | 0.042 (5) | 0.045 (5) | 0.016 (4) | −0.012 (4) | −0.018 (4) |
C3M | 0.060 (5) | 0.041 (5) | 0.051 (5) | 0.018 (4) | −0.010 (4) | −0.022 (4) |
C4M | 0.065 (6) | 0.059 (6) | 0.048 (5) | 0.004 (5) | −0.005 (4) | −0.038 (5) |
C5M | 0.048 (5) | 0.077 (7) | 0.045 (5) | 0.017 (5) | −0.018 (4) | −0.032 (5) |
C6M | 0.039 (4) | 0.050 (5) | 0.034 (4) | 0.015 (4) | −0.010 (3) | −0.023 (4) |
N12 | 0.020 (3) | 0.029 (4) | 0.067 (5) | 0.015 (3) | −0.018 (3) | −0.016 (3) |
C22 | 0.046 (5) | 0.036 (5) | 0.059 (6) | 0.011 (4) | −0.038 (5) | −0.010 (5) |
O22 | 0.048 (4) | 0.076 (5) | 0.053 (4) | 0.020 (3) | −0.020 (3) | −0.031 (4) |
N32 | 0.048 (5) | 0.071 (6) | 0.090 (7) | 0.016 (4) | −0.024 (5) | −0.026 (5) |
C32 | 0.070 (8) | 0.135 (13) | 0.125 (11) | 0.018 (8) | −0.067 (8) | −0.004 (9) |
C42 | 0.037 (5) | 0.044 (6) | 0.104 (9) | 0.006 (4) | −0.022 (5) | −0.018 (6) |
C52 | 0.017 (4) | 0.040 (5) | 0.128 (9) | 0.002 (3) | 0.003 (5) | −0.058 (6) |
C62 | 0.030 (4) | 0.033 (5) | 0.062 (6) | 0.001 (3) | −0.004 (4) | −0.024 (4) |
O62 | 0.046 (3) | 0.053 (4) | 0.068 (4) | 0.006 (3) | 0.003 (3) | −0.032 (3) |
N72 | 0.065 (6) | 0.074 (7) | 0.108 (8) | 0.003 (5) | −0.003 (5) | −0.047 (6) |
C72 | 0.103 (9) | 0.101 (11) | 0.059 (7) | 0.008 (7) | −0.020 (6) | −0.041 (7) |
C82 | 0.073 (7) | 0.060 (7) | 0.131 (11) | 0.036 (6) | −0.063 (8) | −0.045 (8) |
N92 | 0.045 (4) | 0.069 (6) | 0.139 (9) | 0.030 (4) | −0.040 (5) | −0.064 (6) |
Geometric parameters (Å, º) top
Pt1—N11 | 2.079 (5) | C1G—C6G | 1.3900 |
Pt1—P1 | 2.239 (2) | C2G—C3G | 1.3900 |
Pt1—P2 | 2.2697 (18) | C2G—H2G | 0.9500 |
Pt1—Cl1 | 2.340 (2) | C3G—C4G | 1.3900 |
P1—C1C | 1.819 (4) | C3G—H3G | 0.9500 |
P1—C1B | 1.827 (3) | C4G—C5G | 1.3900 |
P1—C1A | 1.849 (3) | C4G—H4G | 0.9500 |
C1A—C2A | 1.3900 | C5G—C6G | 1.3900 |
C1A—C6A | 1.3900 | C5G—H5G | 0.9500 |
C2A—C3A | 1.3900 | C6G—H6G | 0.9500 |
C2A—H2A | 0.9500 | C1H—C6H | 1.3638 |
C3A—C4A | 1.3900 | C1H—C2H | 1.3752 |
C3A—H3A | 0.9500 | C2H—C3H | 1.3964 |
C4A—C5A | 1.3900 | C2H—H2H | 0.9500 |
C4A—H4A | 0.9500 | C3H—C4H | 1.3307 |
C5A—C6A | 1.3900 | C3H—H3H | 0.9500 |
C5A—H5A | 0.9500 | C4H—C5H | 1.3426 |
C6A—H6A | 0.9500 | C4H—H4H | 0.9500 |
C1B—C2B | 1.3900 | C5H—C6H | 1.3937 |
C1B—C6B | 1.3900 | C5H—H5H | 0.9500 |
C2B—C3B | 1.3900 | C6H—H6H | 0.9500 |
C2B—H2B | 0.9500 | C1I—C2I | 1.3900 |
C3B—C4B | 1.3900 | C1I—C6I | 1.3900 |
C3B—H3B | 0.9500 | C2I—C3I | 1.3900 |
C4B—C5B | 1.3900 | C2I—H2I | 0.9500 |
C4B—H4B | 0.9500 | C3I—C4I | 1.3900 |
C5B—C6B | 1.3900 | C3I—H3I | 0.9500 |
C5B—H5B | 0.9500 | C4I—C5I | 1.3900 |
C6B—H6B | 0.9500 | C4I—H4I | 0.9500 |
C1C—C2C | 1.3900 | C5I—C6I | 1.3900 |
C1C—C6C | 1.3900 | C5I—H5I | 0.9500 |
C2C—C3C | 1.3900 | C6I—H6I | 0.9500 |
C2C—H2C | 0.9500 | P4—C1M | 1.839 (4) |
C3C—C4C | 1.3900 | P4—C1L | 1.847 (4) |
C3C—H3C | 0.9500 | P4—C1K | 1.858 (4) |
C4C—C5C | 1.3900 | C1K—C2K | 1.3900 |
C4C—H4C | 0.9500 | C1K—C6K | 1.3900 |
C5C—C6C | 1.3900 | C2K—C3K | 1.3900 |
C5C—H5C | 0.9500 | C2K—H2K | 0.9500 |
C6C—H6C | 0.9500 | C3K—C4K | 1.3900 |
P2—C1D | 1.832 (4) | C3K—H3K | 0.9500 |
P2—C1F | 1.839 (4) | C4K—C5K | 1.3900 |
P2—C1E | 1.839 (4) | C4K—H4K | 0.9500 |
C1D—C2D | 1.3900 | C5K—C6K | 1.3900 |
C1D—C6D | 1.3900 | C5K—H5K | 0.9500 |
C2D—C3D | 1.3900 | C6K—H6K | 0.9500 |
C2D—H2D | 0.9500 | C1L—C2L | 1.3900 |
C3D—C4D | 1.3900 | C1L—C6L | 1.3900 |
C3D—H3D | 0.9500 | C2L—C3L | 1.3900 |
C4D—C5D | 1.3900 | C2L—H2L | 0.9500 |
C4D—H4D | 0.9500 | C3L—C4L | 1.3900 |
C5D—C6D | 1.3900 | C3L—H3L | 0.9500 |
C5D—H5D | 0.9500 | C4L—C5L | 1.3900 |
C6D—H6D | 0.9500 | C4L—H4L | 0.9500 |
C1E—C2E | 1.3900 | C5L—C6L | 1.3900 |
C1E—C6E | 1.3900 | C5L—H5L | 0.9500 |
C2E—C3E | 1.3900 | C6L—H6L | 0.9500 |
C2E—H2E | 0.9500 | C1M—C2M | 1.3900 |
C3E—C4E | 1.3900 | C1M—C6M | 1.3900 |
C3E—H3E | 0.9500 | C2M—C3M | 1.3900 |
C4E—C5E | 1.3900 | C2M—H2M | 0.9500 |
C4E—H4E | 0.9500 | C3M—C4M | 1.3900 |
C5E—C6E | 1.3900 | C3M—H3M | 0.9500 |
C5E—H5E | 0.9500 | C4M—C5M | 1.3900 |
C6E—H6E | 0.9500 | C4M—H4M | 0.9500 |
C1F—C2F | 1.3900 | C5M—C6M | 1.3900 |
C1F—C6F | 1.3900 | C5M—H5M | 0.9500 |
C2F—C3F | 1.3900 | C6M—H6M | 0.9500 |
C2F—H2F | 0.9500 | N12—C62 | 1.362 (8) |
C3F—C4F | 1.3900 | N12—C22 | 1.401 (8) |
C3F—H3F | 0.9500 | C22—O22 | 1.213 (9) |
C4F—C5F | 1.3900 | C22—N32 | 1.407 (8) |
C4F—H4F | 0.9500 | N32—C42 | 1.331 (9) |
C5F—C6F | 1.3900 | N32—C32 | 1.524 (10) |
C5F—H5F | 0.9500 | C32—H32A | 0.9800 |
C6F—H6F | 0.9500 | C32—H32B | 0.9800 |
N11—C61 | 1.369 (7) | C32—H32C | 0.9800 |
N11—C21 | 1.406 (7) | C42—N92 | 1.392 (9) |
C21—O21 | 1.235 (8) | C42—C52 | 1.397 (10) |
C21—N31 | 1.395 (7) | C52—N72 | 1.343 (9) |
N31—C41 | 1.341 (8) | C52—C62 | 1.453 (8) |
N31—C31 | 1.509 (8) | C62—O62 | 1.243 (8) |
C31—H31A | 0.9800 | N72—C82 | 1.395 (10) |
C31—H31B | 0.9800 | N72—C72 | 1.417 (10) |
C31—H31C | 0.9800 | C72—H72A | 0.9800 |
C41—N91 | 1.376 (8) | C72—H72B | 0.9800 |
C41—C51 | 1.401 (8) | C72—H72C | 0.9800 |
C51—N71 | 1.346 (8) | C82—N92 | 1.327 (11) |
C51—C61 | 1.439 (7) | C82—H82 | 0.9500 |
C61—O61 | 1.248 (7) | C45—C43 | 1.512 (15) |
N71—C81 | 1.394 (8) | C45—H45A | 0.9800 |
N71—C71 | 1.433 (8) | C45—H45B | 0.9800 |
C71—H71A | 0.9800 | C45—H45C | 0.9800 |
C71—H71B | 0.9800 | C43—O5 | 1.461 (14) |
C71—H71C | 0.9800 | C43—H43A | 0.9900 |
C81—N91 | 1.356 (9) | C43—H43B | 0.9900 |
C81—H81 | 0.9500 | O5—H5 | 1.118 (14) |
Pt2—N12 | 2.097 (5) | C49—C47 | 1.511 (14) |
Pt2—P3 | 2.251 (2) | C49—H49A | 0.9800 |
Pt2—P4 | 2.2898 (17) | C49—H49B | 0.9800 |
Pt2—Cl2 | 2.349 (2) | C49—H49C | 0.9800 |
P3—C1I | 1.823 (4) | C47—O6 | 1.425 (14) |
P3—C1H | 1.827 (5) | C47—H47A | 0.9900 |
P3—C1G | 1.841 (4) | C47—H47B | 0.9900 |
C1G—C2G | 1.3900 | O6—H6 | 1.121 (14) |
| | | |
N11—Pt1—P1 | 89.67 (19) | C2G—C1G—P3 | 119.9 (3) |
N11—Pt1—P2 | 170.62 (17) | C6G—C1G—P3 | 119.9 (3) |
P1—Pt1—P2 | 98.54 (7) | C1G—C2G—C3G | 120.0 |
N11—Pt1—Cl1 | 86.84 (19) | C1G—C2G—H2G | 120.0 |
P1—Pt1—Cl1 | 175.07 (8) | C3G—C2G—H2G | 120.0 |
P2—Pt1—Cl1 | 85.24 (7) | C2G—C3G—C4G | 120.0 |
C1C—P1—C1B | 110.9 (2) | C2G—C3G—H3G | 120.0 |
C1C—P1—C1A | 100.3 (2) | C4G—C3G—H3G | 120.0 |
C1B—P1—C1A | 104.1 (2) | C5G—C4G—C3G | 120.0 |
C1C—P1—Pt1 | 115.89 (17) | C5G—C4G—H4G | 120.0 |
C1B—P1—Pt1 | 109.99 (16) | C3G—C4G—H4G | 120.0 |
C1A—P1—Pt1 | 114.7 (2) | C6G—C5G—C4G | 120.0 |
C2A—C1A—C6A | 120.0 | C6G—C5G—H5G | 120.0 |
C2A—C1A—P1 | 122.0 (2) | C4G—C5G—H5G | 120.0 |
C6A—C1A—P1 | 118.0 (2) | C5G—C6G—C1G | 120.0 |
C3A—C2A—C1A | 120.0 | C5G—C6G—H6G | 120.0 |
C3A—C2A—H2A | 120.0 | C1G—C6G—H6G | 120.0 |
C1A—C2A—H2A | 120.0 | C6H—C1H—C2H | 118.5 |
C2A—C3A—C4A | 120.0 | C6H—C1H—P3 | 117.1 (4) |
C2A—C3A—H3A | 120.0 | C2H—C1H—P3 | 124.3 (4) |
C4A—C3A—H3A | 120.0 | C1H—C2H—C3H | 118.7 |
C5A—C4A—C3A | 120.0 | C1H—C2H—H2H | 120.7 |
C5A—C4A—H4A | 120.0 | C3H—C2H—H2H | 120.7 |
C3A—C4A—H4A | 120.0 | C4H—C3H—C2H | 122.0 |
C4A—C5A—C6A | 120.0 | C4H—C3H—H3H | 119.0 |
C4A—C5A—H5A | 120.0 | C2H—C3H—H3H | 119.0 |
C6A—C5A—H5A | 120.0 | C3H—C4H—C5H | 119.9 |
C5A—C6A—C1A | 120.0 | C3H—C4H—H4H | 120.1 |
C5A—C6A—H6A | 120.0 | C5H—C4H—H4H | 120.1 |
C1A—C6A—H6A | 120.0 | C4H—C5H—C6H | 119.7 |
C2B—C1B—C6B | 120.0 | C4H—C5H—H5H | 120.2 |
C2B—C1B—P1 | 115.2 (3) | C6H—C5H—H5H | 120.2 |
C6B—C1B—P1 | 124.7 (3) | C1H—C6H—C5H | 121.1 |
C3B—C2B—C1B | 120.0 | C1H—C6H—H6H | 119.4 |
C3B—C2B—H2B | 120.0 | C5H—C6H—H6H | 119.4 |
C1B—C2B—H2B | 120.0 | C2I—C1I—C6I | 120.0 |
C4B—C3B—C2B | 120.0 | C2I—C1I—P3 | 123.8 (3) |
C4B—C3B—H3B | 120.0 | C6I—C1I—P3 | 116.1 (3) |
C2B—C3B—H3B | 120.0 | C1I—C2I—C3I | 120.0 |
C3B—C4B—C5B | 120.0 | C1I—C2I—H2I | 120.0 |
C3B—C4B—H4B | 120.0 | C3I—C2I—H2I | 120.0 |
C5B—C4B—H4B | 120.0 | C2I—C3I—C4I | 120.0 |
C6B—C5B—C4B | 120.0 | C2I—C3I—H3I | 120.0 |
C6B—C5B—H5B | 120.0 | C4I—C3I—H3I | 120.0 |
C4B—C5B—H5B | 120.0 | C3I—C4I—C5I | 120.0 |
C5B—C6B—C1B | 120.0 | C3I—C4I—H4I | 120.0 |
C5B—C6B—H6B | 120.0 | C5I—C4I—H4I | 120.0 |
C1B—C6B—H6B | 120.0 | C4I—C5I—C6I | 120.0 |
C2C—C1C—C6C | 120.0 | C4I—C5I—H5I | 120.0 |
C2C—C1C—P1 | 121.1 (3) | C6I—C5I—H5I | 120.0 |
C6C—C1C—P1 | 118.9 (3) | C5I—C6I—C1I | 120.0 |
C3C—C2C—C1C | 120.0 | C5I—C6I—H6I | 120.0 |
C3C—C2C—H2C | 120.0 | C1I—C6I—H6I | 120.0 |
C1C—C2C—H2C | 120.0 | C1M—P4—C1L | 106.0 (2) |
C2C—C3C—C4C | 120.0 | C1M—P4—C1K | 101.9 (2) |
C2C—C3C—H3C | 120.0 | C1L—P4—C1K | 102.5 (2) |
C4C—C3C—H3C | 120.0 | C1M—P4—Pt2 | 111.81 (16) |
C5C—C4C—C3C | 120.0 | C1L—P4—Pt2 | 113.39 (16) |
C5C—C4C—H4C | 120.0 | C1K—P4—Pt2 | 119.68 (18) |
C3C—C4C—H4C | 120.0 | C2K—C1K—C6K | 120.0 |
C6C—C5C—C4C | 120.0 | C2K—C1K—P4 | 119.3 (3) |
C6C—C5C—H5C | 120.0 | C6K—C1K—P4 | 120.6 (3) |
C4C—C5C—H5C | 120.0 | C3K—C2K—C1K | 120.0 |
C5C—C6C—C1C | 120.0 | C3K—C2K—H2K | 120.0 |
C5C—C6C—H6C | 120.0 | C1K—C2K—H2K | 120.0 |
C1C—C6C—H6C | 120.0 | C2K—C3K—C4K | 120.0 |
C1D—P2—C1F | 108.5 (2) | C2K—C3K—H3K | 120.0 |
C1D—P2—C1E | 103.3 (2) | C4K—C3K—H3K | 120.0 |
C1F—P2—C1E | 101.6 (2) | C5K—C4K—C3K | 120.0 |
C1D—P2—Pt1 | 110.60 (19) | C5K—C4K—H4K | 120.0 |
C1F—P2—Pt1 | 109.14 (16) | C3K—C4K—H4K | 120.0 |
C1E—P2—Pt1 | 122.72 (18) | C4K—C5K—C6K | 120.0 |
C2D—C1D—C6D | 120.0 | C4K—C5K—H5K | 120.0 |
C2D—C1D—P2 | 117.4 (3) | C6K—C5K—H5K | 120.0 |
C6D—C1D—P2 | 122.6 (3) | C5K—C6K—C1K | 120.0 |
C3D—C2D—C1D | 120.0 | C5K—C6K—H6K | 120.0 |
C3D—C2D—H2D | 120.0 | C1K—C6K—H6K | 120.0 |
C1D—C2D—H2D | 120.0 | C2L—C1L—C6L | 120.0 |
C2D—C3D—C4D | 120.0 | C2L—C1L—P4 | 120.5 (2) |
C2D—C3D—H3D | 120.0 | C6L—C1L—P4 | 119.4 (2) |
C4D—C3D—H3D | 120.0 | C1L—C2L—C3L | 120.0 |
C5D—C4D—C3D | 120.0 | C1L—C2L—H2L | 120.0 |
C5D—C4D—H4D | 120.0 | C3L—C2L—H2L | 120.0 |
C3D—C4D—H4D | 120.0 | C4L—C3L—C2L | 120.0 |
C4D—C5D—C6D | 120.0 | C4L—C3L—H3L | 120.0 |
C4D—C5D—H5D | 120.0 | C2L—C3L—H3L | 120.0 |
C6D—C5D—H5D | 120.0 | C3L—C4L—C5L | 120.0 |
C5D—C6D—C1D | 120.0 | C3L—C4L—H4L | 120.0 |
C5D—C6D—H6D | 120.0 | C5L—C4L—H4L | 120.0 |
C1D—C6D—H6D | 120.0 | C4L—C5L—C6L | 120.0 |
C2E—C1E—C6E | 120.0 | C4L—C5L—H5L | 120.0 |
C2E—C1E—P2 | 122.1 (3) | C6L—C5L—H5L | 120.0 |
C6E—C1E—P2 | 117.9 (3) | C5L—C6L—C1L | 120.0 |
C3E—C2E—C1E | 120.0 | C5L—C6L—H6L | 120.0 |
C3E—C2E—H2E | 120.0 | C1L—C6L—H6L | 120.0 |
C1E—C2E—H2E | 120.0 | C2M—C1M—C6M | 120.0 |
C2E—C3E—C4E | 120.0 | C2M—C1M—P4 | 119.4 (3) |
C2E—C3E—H3E | 120.0 | C6M—C1M—P4 | 120.6 (3) |
C4E—C3E—H3E | 120.0 | C3M—C2M—C1M | 120.0 |
C5E—C4E—C3E | 120.0 | C3M—C2M—H2M | 120.0 |
C5E—C4E—H4E | 120.0 | C1M—C2M—H2M | 120.0 |
C3E—C4E—H4E | 120.0 | C2M—C3M—C4M | 120.0 |
C4E—C5E—C6E | 120.0 | C2M—C3M—H3M | 120.0 |
C4E—C5E—H5E | 120.0 | C4M—C3M—H3M | 120.0 |
C6E—C5E—H5E | 120.0 | C5M—C4M—C3M | 120.0 |
C5E—C6E—C1E | 120.0 | C5M—C4M—H4M | 120.0 |
C5E—C6E—H6E | 120.0 | C3M—C4M—H4M | 120.0 |
C1E—C6E—H6E | 120.0 | C6M—C5M—C4M | 120.0 |
C2F—C1F—C6F | 120.0 | C6M—C5M—H5M | 120.0 |
C2F—C1F—P2 | 119.9 (3) | C4M—C5M—H5M | 120.0 |
C6F—C1F—P2 | 120.1 (3) | C5M—C6M—C1M | 120.0 |
C1F—C2F—C3F | 120.0 | C5M—C6M—H6M | 120.0 |
C1F—C2F—H2F | 120.0 | C1M—C6M—H6M | 120.0 |
C3F—C2F—H2F | 120.0 | C62—N12—C22 | 127.2 (5) |
C4F—C3F—C2F | 120.0 | C62—N12—Pt2 | 119.6 (4) |
C4F—C3F—H3F | 120.0 | C22—N12—Pt2 | 112.8 (4) |
C2F—C3F—H3F | 120.0 | O22—C22—N12 | 123.3 (6) |
C3F—C4F—C5F | 120.0 | O22—C22—N32 | 119.0 (7) |
C3F—C4F—H4F | 120.0 | N12—C22—N32 | 117.7 (7) |
C5F—C4F—H4F | 120.0 | C42—N32—C22 | 117.5 (7) |
C6F—C5F—C4F | 120.0 | C42—N32—C32 | 120.6 (7) |
C6F—C5F—H5F | 120.0 | C22—N32—C32 | 120.9 (7) |
C4F—C5F—H5F | 120.0 | N32—C32—H32A | 109.5 |
C5F—C6F—C1F | 120.0 | N32—C32—H32B | 109.5 |
C5F—C6F—H6F | 120.0 | H32A—C32—H32B | 109.5 |
C1F—C6F—H6F | 120.0 | N32—C32—H32C | 109.5 |
C61—N11—C21 | 125.7 (5) | H32A—C32—H32C | 109.5 |
C61—N11—Pt1 | 120.3 (4) | H32B—C32—H32C | 109.5 |
C21—N11—Pt1 | 114.0 (4) | N32—C42—N92 | 121.2 (8) |
O21—C21—N31 | 122.2 (6) | N32—C42—C52 | 124.4 (7) |
O21—C21—N11 | 120.9 (5) | N92—C42—C52 | 114.4 (7) |
N31—C21—N11 | 116.9 (6) | N72—C52—C42 | 104.8 (6) |
C41—N31—C21 | 119.5 (6) | N72—C52—C62 | 134.2 (8) |
C41—N31—C31 | 120.7 (6) | C42—C52—C62 | 120.2 (6) |
C21—N31—C31 | 119.5 (6) | O62—C62—N12 | 120.9 (6) |
N31—C31—H31A | 109.5 | O62—C62—C52 | 126.6 (7) |
N31—C31—H31B | 109.5 | N12—C62—C52 | 112.5 (6) |
H31A—C31—H31B | 109.5 | C52—N72—C82 | 105.2 (7) |
N31—C31—H31C | 109.5 | C52—N72—C72 | 122.5 (8) |
H31A—C31—H31C | 109.5 | C82—N72—C72 | 132.1 (8) |
H31B—C31—H31C | 109.5 | N72—C72—H72A | 109.5 |
N31—C41—N91 | 123.5 (7) | N72—C72—H72B | 109.5 |
N31—C41—C51 | 123.9 (6) | H72A—C72—H72B | 109.5 |
N91—C41—C51 | 112.5 (6) | N72—C72—H72C | 109.5 |
N71—C51—C41 | 106.1 (5) | H72A—C72—H72C | 109.5 |
N71—C51—C61 | 135.2 (6) | H72B—C72—H72C | 109.5 |
C41—C51—C61 | 118.3 (6) | N92—C82—N72 | 116.5 (8) |
O61—C61—N11 | 121.0 (5) | N92—C82—H82 | 121.7 |
O61—C61—C51 | 123.5 (6) | N72—C82—H82 | 121.7 |
N11—C61—C51 | 115.5 (5) | C82—N92—C42 | 99.0 (7) |
C51—N71—C81 | 106.0 (7) | C43—C45—H45A | 109.5 |
C51—N71—C71 | 127.3 (7) | C43—C45—H45B | 109.5 |
C81—N71—C71 | 126.7 (8) | H45A—C45—H45B | 109.5 |
N71—C71—H71A | 109.5 | C43—C45—H45C | 109.5 |
N71—C71—H71B | 109.5 | H45A—C45—H45C | 109.5 |
H71A—C71—H71B | 109.5 | H45B—C45—H45C | 109.5 |
N71—C71—H71C | 109.5 | O5—C43—C45 | 112.1 (19) |
H71A—C71—H71C | 109.5 | O5—C43—H43A | 109.2 |
H71B—C71—H71C | 109.5 | C45—C43—H43A | 109.2 |
N91—C81—N71 | 113.6 (7) | O5—C43—H43B | 109.2 |
N91—C81—H81 | 123.2 | C45—C43—H43B | 109.2 |
N71—C81—H81 | 123.2 | H43A—C43—H43B | 107.9 |
C81—N91—C41 | 101.7 (6) | C43—O5—H5 | 131 (2) |
N12—Pt2—P3 | 88.52 (18) | C47—C49—H49A | 109.5 |
N12—Pt2—P4 | 174.13 (19) | C47—C49—H49B | 109.5 |
P3—Pt2—P4 | 96.96 (7) | H49A—C49—H49B | 109.5 |
N12—Pt2—Cl2 | 84.79 (18) | C47—C49—H49C | 109.5 |
P3—Pt2—Cl2 | 173.03 (7) | H49A—C49—H49C | 109.5 |
P4—Pt2—Cl2 | 89.79 (7) | H49B—C49—H49C | 109.5 |
C1I—P3—C1H | 113.6 (3) | O6—C47—C49 | 121 (2) |
C1I—P3—C1G | 102.1 (2) | O6—C47—H47A | 107.0 |
C1H—P3—C1G | 102.6 (3) | C49—C47—H47A | 107.0 |
C1I—P3—Pt2 | 113.9 (2) | O6—C47—H47B | 107.0 |
C1H—P3—Pt2 | 109.6 (2) | C49—C47—H47B | 107.0 |
C1G—P3—Pt2 | 114.34 (18) | H47A—C47—H47B | 106.8 |
C2G—C1G—C6G | 120.0 | C47—O6—H6 | 133 (2) |
| | | |
N11—Pt1—P1—C1C | −104.7 (2) | N12—Pt2—P3—C1I | −113.3 (3) |
P2—Pt1—P1—C1C | 70.7 (2) | P4—Pt2—P3—C1I | 64.6 (2) |
N11—Pt1—P1—C1B | 128.5 (2) | N12—Pt2—P3—C1H | 118.1 (3) |
P2—Pt1—P1—C1B | −56.07 (18) | P4—Pt2—P3—C1H | −63.9 (2) |
N11—Pt1—P1—C1A | 11.5 (2) | N12—Pt2—P3—C1G | 3.5 (2) |
P2—Pt1—P1—C1A | −173.01 (16) | P4—Pt2—P3—C1G | −178.54 (19) |
C1C—P1—C1A—C2A | −130.1 (3) | C1I—P3—C1G—C2G | −142.8 (3) |
C1B—P1—C1A—C2A | −15.3 (4) | C1H—P3—C1G—C2G | −24.9 (3) |
Pt1—P1—C1A—C2A | 105.0 (3) | Pt2—P3—C1G—C2G | 93.7 (3) |
C1C—P1—C1A—C6A | 53.0 (3) | C1I—P3—C1G—C6G | 42.4 (3) |
C1B—P1—C1A—C6A | 167.8 (3) | C1H—P3—C1G—C6G | 160.3 (3) |
Pt1—P1—C1A—C6A | −71.9 (3) | Pt2—P3—C1G—C6G | −81.0 (3) |
C6A—C1A—C2A—C3A | 0.0 | C6G—C1G—C2G—C3G | 0.0 |
P1—C1A—C2A—C3A | −176.8 (4) | P3—C1G—C2G—C3G | −174.7 (4) |
C1A—C2A—C3A—C4A | 0.0 | C1G—C2G—C3G—C4G | 0.0 |
C2A—C3A—C4A—C5A | 0.0 | C2G—C3G—C4G—C5G | 0.0 |
C3A—C4A—C5A—C6A | 0.0 | C3G—C4G—C5G—C6G | 0.0 |
C4A—C5A—C6A—C1A | 0.0 | C4G—C5G—C6G—C1G | 0.0 |
C2A—C1A—C6A—C5A | 0.0 | C2G—C1G—C6G—C5G | 0.0 |
P1—C1A—C6A—C5A | 176.9 (4) | P3—C1G—C6G—C5G | 174.7 (4) |
C1C—P1—C1B—C2B | −177.4 (3) | C1I—P3—C1H—C6H | −150.0 (4) |
C1A—P1—C1B—C2B | 75.5 (3) | C1G—P3—C1H—C6H | 100.6 (4) |
Pt1—P1—C1B—C2B | −47.8 (3) | Pt2—P3—C1H—C6H | −21.3 (5) |
C1C—P1—C1B—C6B | 6.5 (4) | C1I—P3—C1H—C2H | 32.7 (6) |
C1A—P1—C1B—C6B | −100.6 (3) | C1G—P3—C1H—C2H | −76.7 (5) |
Pt1—P1—C1B—C6B | 136.1 (2) | Pt2—P3—C1H—C2H | 161.4 (4) |
C6B—C1B—C2B—C3B | 0.0 | C6H—C1H—C2H—C3H | 0.3 |
P1—C1B—C2B—C3B | −176.3 (3) | P3—C1H—C2H—C3H | 177.6 (6) |
C1B—C2B—C3B—C4B | 0.0 | C1H—C2H—C3H—C4H | 1.7 |
C2B—C3B—C4B—C5B | 0.0 | C2H—C3H—C4H—C5H | −3.2 |
C3B—C4B—C5B—C6B | 0.0 | C3H—C4H—C5H—C6H | 2.5 |
C4B—C5B—C6B—C1B | 0.0 | C2H—C1H—C6H—C5H | −1.0 |
C2B—C1B—C6B—C5B | 0.0 | P3—C1H—C6H—C5H | −178.4 (5) |
P1—C1B—C6B—C5B | 175.9 (4) | C4H—C5H—C6H—C1H | −0.4 |
C1B—P1—C1C—C2C | −47.7 (4) | C1H—P3—C1I—C2I | −41.8 (4) |
C1A—P1—C1C—C2C | 61.9 (3) | C1G—P3—C1I—C2I | 67.9 (4) |
Pt1—P1—C1C—C2C | −174.0 (2) | Pt2—P3—C1I—C2I | −168.3 (3) |
C1B—P1—C1C—C6C | 131.9 (3) | C1H—P3—C1I—C6I | 141.6 (3) |
C1A—P1—C1C—C6C | −118.5 (3) | C1G—P3—C1I—C6I | −108.6 (3) |
Pt1—P1—C1C—C6C | 5.5 (3) | Pt2—P3—C1I—C6I | 15.1 (3) |
C6C—C1C—C2C—C3C | 0.0 | C6I—C1I—C2I—C3I | 0.0 |
P1—C1C—C2C—C3C | 179.6 (4) | P3—C1I—C2I—C3I | −176.4 (4) |
C1C—C2C—C3C—C4C | 0.0 | C1I—C2I—C3I—C4I | 0.0 |
C2C—C3C—C4C—C5C | 0.0 | C2I—C3I—C4I—C5I | 0.0 |
C3C—C4C—C5C—C6C | 0.0 | C3I—C4I—C5I—C6I | 0.0 |
C4C—C5C—C6C—C1C | 0.0 | C4I—C5I—C6I—C1I | 0.0 |
C2C—C1C—C6C—C5C | 0.0 | C2I—C1I—C6I—C5I | 0.0 |
P1—C1C—C6C—C5C | −179.6 (4) | P3—C1I—C6I—C5I | 176.7 (4) |
P1—Pt1—P2—C1D | 127.2 (2) | P3—Pt2—P4—C1M | −128.39 (19) |
Cl1—Pt1—P2—C1D | −49.6 (2) | Cl2—Pt2—P4—C1M | 53.34 (19) |
P1—Pt1—P2—C1F | −113.4 (2) | P3—Pt2—P4—C1L | 111.8 (2) |
Cl1—Pt1—P2—C1F | 69.8 (2) | Cl2—Pt2—P4—C1L | −66.5 (2) |
P1—Pt1—P2—C1E | 4.99 (19) | P3—Pt2—P4—C1K | −9.5 (2) |
Cl1—Pt1—P2—C1E | −171.81 (19) | Cl2—Pt2—P4—C1K | 172.3 (2) |
C1F—P2—C1D—C2D | −169.5 (3) | C1M—P4—C1K—C2K | 30.7 (3) |
C1E—P2—C1D—C2D | 83.2 (4) | C1L—P4—C1K—C2K | 140.3 (3) |
Pt1—P2—C1D—C2D | −49.8 (4) | Pt2—P4—C1K—C2K | −93.2 (3) |
C1F—P2—C1D—C6D | 10.4 (4) | C1M—P4—C1K—C6K | −150.7 (3) |
C1E—P2—C1D—C6D | −96.9 (4) | C1L—P4—C1K—C6K | −41.1 (3) |
Pt1—P2—C1D—C6D | 130.1 (3) | Pt2—P4—C1K—C6K | 85.4 (3) |
C6D—C1D—C2D—C3D | 0.0 | C6K—C1K—C2K—C3K | 0.0 |
P2—C1D—C2D—C3D | 179.9 (4) | P4—C1K—C2K—C3K | 178.6 (4) |
C1D—C2D—C3D—C4D | 0.0 | C1K—C2K—C3K—C4K | 0.0 |
C2D—C3D—C4D—C5D | 0.0 | C2K—C3K—C4K—C5K | 0.0 |
C3D—C4D—C5D—C6D | 0.0 | C3K—C4K—C5K—C6K | 0.0 |
C4D—C5D—C6D—C1D | 0.0 | C4K—C5K—C6K—C1K | 0.0 |
C2D—C1D—C6D—C5D | 0.0 | C2K—C1K—C6K—C5K | 0.0 |
P2—C1D—C6D—C5D | −179.9 (5) | P4—C1K—C6K—C5K | −178.6 (4) |
C1D—P2—C1E—C2E | −22.2 (3) | C1M—P4—C1L—C2L | 69.4 (4) |
C1F—P2—C1E—C2E | −134.6 (3) | C1K—P4—C1L—C2L | −37.1 (4) |
Pt1—P2—C1E—C2E | 103.4 (3) | Pt2—P4—C1L—C2L | −167.5 (3) |
C1D—P2—C1E—C6E | 158.7 (3) | C1M—P4—C1L—C6L | −108.9 (3) |
C1F—P2—C1E—C6E | 46.3 (3) | C1K—P4—C1L—C6L | 144.6 (3) |
Pt1—P2—C1E—C6E | −75.7 (3) | Pt2—P4—C1L—C6L | 14.1 (4) |
C6E—C1E—C2E—C3E | 0.0 | C6L—C1L—C2L—C3L | 0.0 |
P2—C1E—C2E—C3E | −179.1 (4) | P4—C1L—C2L—C3L | −178.3 (4) |
C1E—C2E—C3E—C4E | 0.0 | C1L—C2L—C3L—C4L | 0.0 |
C2E—C3E—C4E—C5E | 0.0 | C2L—C3L—C4L—C5L | 0.0 |
C3E—C4E—C5E—C6E | 0.0 | C3L—C4L—C5L—C6L | 0.0 |
C4E—C5E—C6E—C1E | 0.0 | C4L—C5L—C6L—C1L | 0.0 |
C2E—C1E—C6E—C5E | 0.0 | C2L—C1L—C6L—C5L | 0.0 |
P2—C1E—C6E—C5E | 179.1 (4) | P4—C1L—C6L—C5L | 178.3 (4) |
C1D—P2—C1F—C2F | −65.0 (4) | C1L—P4—C1M—C2M | −47.0 (3) |
C1E—P2—C1F—C2F | 43.4 (4) | C1K—P4—C1M—C2M | 60.0 (3) |
Pt1—P2—C1F—C2F | 174.4 (3) | Pt2—P4—C1M—C2M | −171.0 (2) |
C1D—P2—C1F—C6F | 116.4 (4) | C1L—P4—C1M—C6M | 131.7 (3) |
C1E—P2—C1F—C6F | −135.1 (3) | C1K—P4—C1M—C6M | −121.3 (3) |
Pt1—P2—C1F—C6F | −4.2 (4) | Pt2—P4—C1M—C6M | 7.7 (3) |
C6F—C1F—C2F—C3F | 0.0 | C6M—C1M—C2M—C3M | 0.0 |
P2—C1F—C2F—C3F | −178.6 (4) | P4—C1M—C2M—C3M | 178.7 (4) |
C1F—C2F—C3F—C4F | 0.0 | C1M—C2M—C3M—C4M | 0.0 |
C2F—C3F—C4F—C5F | 0.0 | C2M—C3M—C4M—C5M | 0.0 |
C3F—C4F—C5F—C6F | 0.0 | C3M—C4M—C5M—C6M | 0.0 |
C4F—C5F—C6F—C1F | 0.0 | C4M—C5M—C6M—C1M | 0.0 |
C2F—C1F—C6F—C5F | 0.0 | C2M—C1M—C6M—C5M | 0.0 |
P2—C1F—C6F—C5F | 178.6 (4) | P4—C1M—C6M—C5M | −178.7 (4) |
P1—Pt1—N11—C61 | −83.3 (6) | P3—Pt2—N12—C62 | −85.0 (6) |
Cl1—Pt1—N11—C61 | 93.2 (6) | Cl2—Pt2—N12—C62 | 93.1 (6) |
P1—Pt1—N11—C21 | 94.5 (5) | P3—Pt2—N12—C22 | 88.8 (5) |
Cl1—Pt1—N11—C21 | −89.0 (5) | Cl2—Pt2—N12—C22 | −93.2 (5) |
C61—N11—C21—O21 | 176.2 (8) | C62—N12—C22—O22 | 175.3 (9) |
Pt1—N11—C21—O21 | −1.4 (10) | Pt2—N12—C22—O22 | 2.1 (11) |
C61—N11—C21—N31 | −0.7 (12) | C62—N12—C22—N32 | −4.8 (13) |
Pt1—N11—C21—N31 | −178.3 (6) | Pt2—N12—C22—N32 | −178.0 (6) |
O21—C21—N31—C41 | −173.3 (9) | O22—C22—N32—C42 | −173.4 (9) |
N11—C21—N31—C41 | 3.6 (12) | N12—C22—N32—C42 | 6.7 (13) |
O21—C21—N31—C31 | 0.0 (14) | O22—C22—N32—C32 | −4.7 (15) |
N11—C21—N31—C31 | 176.8 (8) | N12—C22—N32—C32 | 175.4 (9) |
C21—N31—C41—N91 | 175.9 (9) | C22—N32—C42—N92 | 171.8 (9) |
C31—N31—C41—N91 | 2.8 (16) | C32—N32—C42—N92 | 3.1 (15) |
C21—N31—C41—C51 | −6.6 (14) | C22—N32—C42—C52 | −7.5 (15) |
C31—N31—C41—C51 | −179.7 (9) | C32—N32—C42—C52 | −176.2 (9) |
N31—C41—C51—N71 | 179.4 (9) | N32—C42—C52—N72 | 176.8 (10) |
N91—C41—C51—N71 | −2.9 (12) | N92—C42—C52—N72 | −2.6 (11) |
N31—C41—C51—C61 | 6.2 (14) | N32—C42—C52—C62 | 5.6 (15) |
N91—C41—C51—C61 | −176.0 (9) | N92—C42—C52—C62 | −173.7 (8) |
C21—N11—C61—O61 | −178.7 (7) | C22—N12—C62—O62 | −177.0 (8) |
Pt1—N11—C61—O61 | −1.3 (10) | Pt2—N12—C62—O62 | −4.3 (11) |
C21—N11—C61—C51 | 0.5 (12) | C22—N12—C62—C52 | 2.7 (12) |
Pt1—N11—C61—C51 | 177.9 (5) | Pt2—N12—C62—C52 | 175.5 (5) |
N71—C51—C61—O61 | 5.6 (16) | N72—C52—C62—O62 | 8.9 (16) |
C41—C51—C61—O61 | 176.2 (8) | C42—C52—C62—O62 | 176.9 (8) |
N71—C51—C61—N11 | −173.6 (10) | N72—C52—C62—N12 | −170.8 (10) |
C41—C51—C61—N11 | −2.9 (11) | C42—C52—C62—N12 | −2.8 (12) |
C41—C51—N71—C81 | 2.3 (11) | C42—C52—N72—C82 | 2.9 (11) |
C61—C51—N71—C81 | 173.7 (11) | C62—C52—N72—C82 | 172.3 (10) |
C41—C51—N71—C71 | −179.0 (10) | C42—C52—N72—C72 | −173.5 (10) |
C61—C51—N71—C71 | −7.6 (18) | C62—C52—N72—C72 | −4.2 (17) |
C51—N71—C81—N91 | −1.1 (15) | C52—N72—C82—N92 | −2.7 (14) |
C71—N71—C81—N91 | −179.8 (11) | C72—N72—C82—N92 | 173.2 (12) |
N71—C81—N91—C41 | −0.6 (15) | N72—C82—N92—C42 | 1.1 (13) |
N31—C41—N91—C81 | 179.9 (11) | N32—C42—N92—C82 | −178.5 (10) |
C51—C41—N91—C81 | 2.1 (13) | C52—C42—N92—C82 | 0.9 (12) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O61 | 1.12 (1) | 2.13 (2) | 2.74 (2) | 111 (2) |
O6—H6···O21 | 1.12 (1) | 2.43 (2) | 3.089 (17) | 116 (2) |
C3A—H3A···Cl2 | 0.95 | 2.83 | 3.549 (4) | 133 |
C3G—H3G···O21i | 0.95 | 2.54 | 3.469 (7) | 167 |
C5E—H5E···Cl2ii | 0.95 | 2.81 | 3.511 (5) | 131 |
C5I—H5I···O22iii | 0.95 | 2.21 | 3.129 (8) | 162 |
C6L—H6L···Cl2 | 0.95 | 2.73 | 3.428 (5) | 131 |
C49—H49C···O61iv | 0.98 | 2.38 | 2.94 (3) | 116 |
C72—H72B···Cl1i | 0.98 | 2.78 | 3.571 (13) | 138 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) −x+2, −y+1, −z; (iv) x−1, y, z. |
Experimental details
| (I) | (II) |
Crystal data |
Chemical formula | [Pt(C7H7N4O2)2(C18H15P)2] | [PtCl(C7H7N4O2)(C18H15P)2]·0.5C2H6O |
Mr | 1077.96 | 957.28 |
Crystal system, space group | Monoclinic, P21/c | Triclinic, P1 |
Temperature (K) | 183 | 183 |
a, b, c (Å) | 9.7839 (5), 20.7991 (10), 22.0788 (12) | 11.4777 (9), 19.3276 (13), 20.5946 (17) |
α, β, γ (°) | 90, 99.172 (6), 90 | 62.565 (8), 81.354 (10), 89.019 (9) |
V (Å3) | 4435.5 (4) | 4001.7 (5) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 3.29 | 3.70 |
Crystal size (mm) | 0.27 × 0.16 × 0.08 | 0.36 × 0.18 × 0.06 |
|
Data collection |
Diffractometer | Stoe IPDS diffractometer | Stoe IPDS diffractometer |
Absorption correction | Numerical (Coppens et al., 1965) | Numerical (Coppens et al., 1965) |
Tmin, Tmax | 0.470, 0.779 | 0.350, 0.809 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 52916, 13203, 9092 | 43394, 19993, 8805 |
Rint | 0.067 | 0.096 |
(sin θ/λ)max (Å−1) | 0.710 | 0.689 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.084, 1.01 | 0.042, 0.092, 0.69 |
No. of reflections | 13203 | 19993 |
No. of parameters | 585 | 839 |
No. of restraints | 0 | 59 |
H-atom treatment | H-atom parameters constrained | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.42, −3.35 | 1.40, −2.62 |
Selected geometric parameters (Å, º) for (I) topPt—N71 | 2.069 (3) | N71—C81 | 1.315 (6) |
Pt—N72 | 2.071 (3) | C81—N91 | 1.341 (6) |
Pt—P2 | 2.2685 (11) | N12—C22 | 1.402 (7) |
Pt—P1 | 2.2792 (11) | N12—C62 | 1.412 (6) |
N11—C21 | 1.401 (6) | N12—C12 | 1.482 (6) |
N11—C61 | 1.412 (6) | C22—O22 | 1.226 (6) |
N11—C11 | 1.476 (7) | C22—N32 | 1.374 (6) |
C21—O21 | 1.225 (6) | N32—C42 | 1.390 (6) |
C21—N31 | 1.377 (7) | N32—C32 | 1.460 (6) |
N31—C41 | 1.391 (6) | C42—N92 | 1.356 (6) |
N31—C31 | 1.462 (6) | C42—C52 | 1.370 (6) |
C41—N91 | 1.349 (6) | C52—N72 | 1.390 (5) |
C41—C51 | 1.378 (6) | C52—C62 | 1.423 (6) |
C51—N71 | 1.395 (5) | C62—O62 | 1.231 (6) |
C51—C61 | 1.415 (6) | N72—C82 | 1.326 (5) |
C61—O61 | 1.233 (6) | C82—N92 | 1.375 (6) |
| | | |
N71—Pt—N72 | 87.05 (14) | C21—N31—C41 | 119.2 (4) |
N71—Pt—P2 | 174.37 (10) | C81—N71—C51 | 104.0 (3) |
N72—Pt—P2 | 87.88 (10) | C81—N91—C41 | 102.0 (4) |
N71—Pt—P1 | 87.60 (10) | C22—N12—C62 | 126.9 (4) |
N72—Pt—P1 | 174.04 (11) | C22—N32—C42 | 118.9 (4) |
P2—Pt—P1 | 97.57 (4) | C82—N72—C52 | 104.8 (3) |
C21—N11—C61 | 126.1 (4) | C42—N92—C82 | 101.7 (4) |
Hydrogen-bond geometry (Å, º) for (I) top
D—H···A | D—H | H···A | D···A | D—H···A |
C4B—H4B···O21i | 0.95 | 2.42 | 3.065 (6) | 125 |
C10A—H10A···O22ii | 0.95 | 2.51 | 3.184 (6) | 128 |
Symmetry codes: (i) x+1, −y+1/2, z+1/2; (ii) −x+2, y−1/2, −z+3/2. |
Selected geometric parameters (Å, º) for (II) topPt1—N11 | 2.079 (5) | Pt2—N12 | 2.097 (5) |
Pt1—P1 | 2.239 (2) | Pt2—P3 | 2.251 (2) |
Pt1—P2 | 2.2697 (18) | Pt2—P4 | 2.2898 (17) |
Pt1—Cl1 | 2.340 (2) | Pt2—Cl2 | 2.349 (2) |
N11—C61 | 1.369 (7) | N12—C62 | 1.362 (8) |
N11—C21 | 1.406 (7) | N12—C22 | 1.401 (8) |
C21—O21 | 1.235 (8) | C22—O22 | 1.213 (9) |
C21—N31 | 1.395 (7) | C22—N32 | 1.407 (8) |
N31—C41 | 1.341 (8) | N32—C42 | 1.331 (9) |
N31—C31 | 1.509 (8) | N32—C32 | 1.524 (10) |
C41—N91 | 1.376 (8) | C42—N92 | 1.392 (9) |
C41—C51 | 1.401 (8) | C42—C52 | 1.397 (10) |
C51—N71 | 1.346 (8) | C52—N72 | 1.343 (9) |
C51—C61 | 1.439 (7) | C52—C62 | 1.453 (8) |
C61—O61 | 1.248 (7) | C62—O62 | 1.243 (8) |
N71—C81 | 1.394 (8) | N72—C82 | 1.395 (10) |
N71—C71 | 1.433 (8) | N72—C72 | 1.417 (10) |
C81—N91 | 1.356 (9) | C82—N92 | 1.327 (11) |
| | | |
N11—Pt1—P1 | 89.67 (19) | N12—Pt2—P3 | 88.52 (18) |
N11—Pt1—P2 | 170.62 (17) | N12—Pt2—P4 | 174.13 (19) |
P1—Pt1—P2 | 98.54 (7) | P3—Pt2—P4 | 96.96 (7) |
N11—Pt1—Cl1 | 86.84 (19) | N12—Pt2—Cl2 | 84.79 (18) |
P1—Pt1—Cl1 | 175.07 (8) | P3—Pt2—Cl2 | 173.03 (7) |
P2—Pt1—Cl1 | 85.24 (7) | P4—Pt2—Cl2 | 89.79 (7) |
C61—N11—C21 | 125.7 (5) | C62—N12—C22 | 127.2 (5) |
C41—N31—C21 | 119.5 (6) | C42—N32—C22 | 117.5 (7) |
C51—N71—C81 | 106.0 (7) | C52—N72—C82 | 105.2 (7) |
C81—N91—C41 | 101.7 (6) | C82—N92—C42 | 99.0 (7) |
Hydrogen-bond geometry (Å, º) for (II) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O61 | 1.118 (14) | 2.13 (2) | 2.74 (2) | 111 (2) |
O6—H6···O21 | 1.121 (14) | 2.43 (2) | 3.089 (17) | 115.7 (19) |
C3A—H3A···Cl2 | 0.95 | 2.83 | 3.549 (4) | 133 |
C3G—H3G···O21i | 0.95 | 2.54 | 3.469 (7) | 167 |
C5E—H5E···Cl2ii | 0.95 | 2.81 | 3.511 (5) | 131 |
C5I—H5I···O22iii | 0.95 | 2.21 | 3.129 (8) | 162 |
C6L—H6L···Cl2 | 0.95 | 2.73 | 3.428 (5) | 131 |
C49—H49C···O61iv | 0.98 | 2.38 | 2.94 (3) | 116 |
C72—H72B···Cl1i | 0.98 | 2.78 | 3.571 (13) | 138 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) −x+2, −y+1, −z; (iv) x−1, y, z. |
Transition metal complexes of nucleobase derivatives may serve as models for the coordination of metals to nucleic acids. The methylated oxopurines theophylline and theobromine are of additional interest in view of their pharmacological properties. Theophylline exhibits anti-asthmatic effects, theobromine is in current clinical use as a vasodilator and a bronchodilator, and both oxopurines are also used as cardiac stimulants or muscle relaxants. Pt complexes of these oxopurines may be worthy of additional attention because of the potential antitumour activity of such complexes (Bloemink & Reedijk, 1996; Whitehead & Lippard, 1996). We here report the synthesis and structure of two molecular platinum(II) complexes involving triphenylphosphine and the anions of theophylline (TP) and theobromine (TB) as ligands, respectively, namely cis-[Pt(TP-)2(PPh3)2], (I), and cis-[PtCl(TB-)(PPh3)2]·0.5EtOH, (II). \sch
In metal complexes synthesized in non-alkaline media, theophylline binds as a neutral ligand, whereas complexes crystallized from alkaline solutions show the presence of theophyllinate anions (Madarasz et al., 2000), usually deprotonated at N7, the atom where the H atom is located in the crystal structure of neutral theophylline (Ebisuzaki et al., 1997), and single-crystal data for many metal complexes prove that theophylline moieties are normally bonded to the metal centre through N7 (Madarasz et al., 2000). There are, however, some rare examples of other coordination modes of unsubstituted theophylline or theophyllinate anions. N7 coordination including a balanced metal-O6 chelation has been found in a titanium cyclopentadienyl complex, with a Ti—O6 distance of 2.28 Å (Cozak et al., 1986), whereas some weak N7/O6 chelating interactions have been established, for example in copper(II) complexes, with a Cu—O6 distance of 2.92 Å (Szalda et al., 1976), or of 3.34 Å (Kistenmacher et al., 1978; Madarasz et al., 2000). N9 coordination of theophyllinate anions, in spite of steric hindrance by the neighbouring methyl group at N3, has been established in a dimeric rhodium(II) complex (Aoki & Yamazaki, 1980), whereas neutral theophylline also bonds through N9 in a chloroplatinum(II) complex (Griffith & Amma, 1979). N7/N9 bridging theophyllinate anions, including a weak Pt—O6 interaction of 2.34 Å, have been observed in a hexameric trimethylplatinum complex (Lorberth et al., 1988). Finally, in a mixed ligand PdII complex, theophyllinate anions are linked to the metal through C8 (Romerosa et al., 1997).
The molecular structure of (I) is shown in Fig. 1. Two theophyllinate monoanions indeed coordinate to PtII via the N7 atoms. Compound (I) exhibits a slightly distorted square-planar coordination geometry around Pt, with two N7-coordinating theophyllinate anions [Pt—N71 2.069 (3) and Pt—N72 2.071 (3) Å] and two P atoms from the triphenylphosphine groups [Pt—P1 2.2792 (11) and Pt—P2 2.2685 (11) Å] in a cis arrangement (Fig. 1). Weak C—H···O hydrogen-bonding interactions are observed involving O2, with donor-acceptor distances of 3.065 (6) and 3.184 (6) Å. Two rather close contacts are observed between Pt and atoms O61 and O62 adjacent to N71 and N72, with Pt···O61 and Pt···O62 distances of 3.234 (4) and 3.284 (4) Å, respectively.
In theobromine, in contrast with theophylline, the N7 coordination site is blocked by a methyl group, and therefore N9 is expected to be the preferred coordination site. Such a coordination is found in the only theobromine metal complex structure reported to date, K[PtII(TB)Cl3] (Crowston et al., 1986). In complex (II), however, we have now established a structure involving theobrominate anions coordinating to Pt through N1 in both crystallographically independent molecules. In addition, one Cl- anion and two cis P atoms from triphenylphosphine groups are coordinated to Pt, forming a slightly distorted square-planar coordination geometry (Fig. 3). The metal-ligand distances in molecules 1 and 2, respectively, are Pt1—N11 2.079 (5) and Pt2—N12 2.097 (5), Pt1—Cl1 2.340 (2) and Pt2—Cl2 2.349 (2), Pt1—P1 2.239 (2) and Pt1—P2 2.2697 (18), and Pt2—P3 2.251 (2) and Pt2—P4 2.2898 (17) Å. The Pt—P distances in (II) trans to the purine ligands are significantly longer (by about 0.04 Å) than the corresponding values trans to the Cl atoms in both crystallographically independent molecules: the purine base obviously exhibits a stronger trans influence than the Cl atom.
In both complexes, the Pt—N(purine) distances are significantly longer than in corresponding complexes without triphenylphosphine ligands. This fact may be explained by a lengthening of the Pt—N bonds due to the relatively high trans influence of PPh3.
The heterocyclic oxopurine rings are rotated with respect to the coordination plane of the metal by 82.99 (8) and 88.09 (8)° in complex (I), and by 85.91 (16) and 88.14 (18)° in complex (II). The maximum deviations of individual purine ring atoms from the least-squares plane through the nine ring atoms are 0.040 (4) Å for N12 in (I) and 0.077 (8) for C52 in (II), whereas the corresponding maximum deviations for ring-substituent atoms are 0.256 (7) Å for C32 in (I) and 0.17 (1) Å for O22 in (II).
In both complexes, the structures are stabilized by intramolecular stacking interactions between the purine rings and a phenyl ring of an adjacent triphenylphosphine group (Figs. 2 and 4). The corresponding stacking distances (calculated as the mean distance of all ring atoms of one molecule from the least-squares planes through the stacking molecule) and stacking angles are 3.26 Å and 10.0°, respectively, for molecule 1, and 3.32 Å and 13.7°, respectively, for molecule 2 in the theophylline complex, (I). In the theobromine complex, (II), the corresponding values are 3.31 Å and 19.9°, respectively, for molecule 1, and 3.32 Å and 12.0°, respectively, for molecule 2. The hydrogen-bonding contacts for (II) are shown in Fig. 3 and Table 4.