


Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680801533X/si2089sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S160053680801533X/si2089Isup2.hkl |
CCDC reference: 696416
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean
(C-C) = 0.006 Å
- R factor = 0.040
- wR factor = 0.069
- Data-to-parameter ratio = 18.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT214_ALERT_2_C Atom C43 (Anion/Solvent) ADP max/min Ratio 4.60 prola PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.12 Ratio PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT180_ALERT_4_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C H4 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C H4 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 N O3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
All reactions were carried out under an atmosphere of dry nitrogen using standard Schlenk techniques. Solvents were dried and stored under nitrogen. Platinum(II)nitrate was purchased from ChemPur and Tris(2-(diphenylphosphino)ethyl)-phosphine was obtained from Acros Organics.
150 mg (0.47 mmol) Platinum(II)nitrate was dissolved in 50 ml water and 50 ml e thanol was added. 315 mg (0.47 mmol) Tris(2-(diphenylphosphino)ethyl)- phosphine (PP3) was dissolved in dichlormethane and added to the reaction mixture. The suspension was stirred at room temperature for 3 days. Afterwards the mixture was concentrated to small volume and a yellow solid precipitated. The precipitate was filtered and dried in vacuo. Single crystals were received by gas phase diffusion of diethyl ether into a solution of the yellow product in methanol.
All non-hydrogen atoms were refined anisotropically and H atoms were refined using riding constraints with C—H distances set to 0.95 Å for aromatic, to 0.99 Å for aliphatic, 0.98 Å for methanol C—H bonds and 0.84 Å for O—H bonds. Uiso(H) values were set to 1.2 Ueq of the parent atom.
Data collection: SMART (Bruker, 2000); cell refinement: SMART (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
![]() | Fig. 1. ORTEP representation of the PtII complex with displacement ellipsoids at 50% probability. H atoms and labels for symmetry equivalent C atoms have been omitted for clarity. |
[Pt(NO3)2(C42H42O2P4)2]·4CH4O | Z = 1 |
Mr = 1852.64 | F(000) = 952 |
Triclinic, P1 | Dx = 1.419 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.9905 (9) Å | Cell parameters from 5288 reflections |
b = 14.3346 (13) Å | θ = 4.9–49.4° |
c = 16.9916 (15) Å | µ = 1.83 mm−1 |
α = 66.200 (1)° | T = 153 K |
β = 77.479 (1)° | Plate, colourless |
γ = 88.477 (1)° | 0.48 × 0.10 × 0.03 mm |
V = 2168.4 (3) Å3 |
Bruker SMART APEX CCD area-detector diffractometer | 9347 independent reflections |
Radiation source: fine-focus sealed tube | 8160 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
ϕ and ω scans | θmax = 27.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1995) | h = −12→12 |
Tmin = 0.474, Tmax = 0.947 | k = −18→18 |
25181 measured reflections | l = −21→21 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.068 | H-atom parameters constrained |
S = 0.91 | w = 1/[σ2(Fo2) + (0.0185P)2] where P = (Fo2 + 2Fc2)/3 |
9347 reflections | (Δ/σ)max < 0.001 |
512 parameters | Δρmax = 1.31 e Å−3 |
0 restraints | Δρmin = −1.37 e Å−3 |
[Pt(NO3)2(C42H42O2P4)2]·4CH4O | γ = 88.477 (1)° |
Mr = 1852.64 | V = 2168.4 (3) Å3 |
Triclinic, P1 | Z = 1 |
a = 9.9905 (9) Å | Mo Kα radiation |
b = 14.3346 (13) Å | µ = 1.83 mm−1 |
c = 16.9916 (15) Å | T = 153 K |
α = 66.200 (1)° | 0.48 × 0.10 × 0.03 mm |
β = 77.479 (1)° |
Bruker SMART APEX CCD area-detector diffractometer | 9347 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1995) | 8160 reflections with I > 2σ(I) |
Tmin = 0.474, Tmax = 0.947 | Rint = 0.052 |
25181 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 0 restraints |
wR(F2) = 0.068 | H-atom parameters constrained |
S = 0.91 | Δρmax = 1.31 e Å−3 |
9347 reflections | Δρmin = −1.37 e Å−3 |
512 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Pt1 | 0.0000 | 0.0000 | 0.0000 | 0.01742 (6) | |
P1 | 0.18605 (9) | 0.10153 (7) | −0.00768 (6) | 0.0217 (2) | |
P2 | 0.14224 (9) | −0.01106 (7) | −0.12330 (6) | 0.0210 (2) | |
P3 | 0.24812 (10) | −0.28401 (7) | −0.17502 (6) | 0.0255 (2) | |
P4 | 0.09161 (11) | 0.23615 (7) | −0.36073 (6) | 0.0293 (2) | |
N1 | −0.3437 (4) | 0.2080 (3) | −0.0989 (3) | 0.0416 (9) | |
O1 | 0.1078 (2) | −0.29710 (18) | −0.18776 (16) | 0.0335 (6) | |
O2 | 0.2424 (3) | 0.23539 (19) | −0.39496 (16) | 0.0390 (7) | |
O3 | −0.3782 (3) | 0.2601 (3) | −0.1679 (2) | 0.1131 (17) | |
O4 | −0.2262 (3) | 0.1769 (2) | −0.10285 (19) | 0.0493 (8) | |
O5 | −0.4257 (3) | 0.1826 (2) | −0.02587 (19) | 0.0424 (7) | |
C1 | 0.3381 (3) | 0.0626 (3) | −0.0654 (2) | 0.0253 (8) | |
H1B | 0.4176 | 0.1115 | −0.0810 | 0.030* | |
H1C | 0.3608 | −0.0060 | −0.0269 | 0.030* | |
C2 | 0.3073 (3) | 0.0605 (3) | −0.1490 (2) | 0.0266 (9) | |
H2B | 0.3817 | 0.0281 | −0.1757 | 0.032* | |
H2C | 0.3040 | 0.1313 | −0.1924 | 0.032* | |
C3 | 0.1821 (3) | −0.1423 (2) | −0.1047 (2) | 0.0237 (8) | |
H3A | 0.2208 | −0.1713 | −0.0515 | 0.028* | |
H3B | 0.0949 | −0.1825 | −0.0916 | 0.028* | |
C4 | 0.2830 (4) | −0.1576 (2) | −0.1808 (2) | 0.0271 (9) | |
H4A | 0.3787 | −0.1501 | −0.1760 | 0.032* | |
H4B | 0.2720 | −0.1051 | −0.2382 | 0.032* | |
C5 | 0.0837 (4) | 0.0428 (2) | −0.2265 (2) | 0.0247 (8) | |
H5A | 0.1591 | 0.0444 | −0.2757 | 0.030* | |
H5B | 0.0058 | −0.0013 | −0.2227 | 0.030* | |
C6 | 0.0380 (4) | 0.1520 (3) | −0.2456 (2) | 0.0287 (9) | |
H6A | 0.0774 | 0.1798 | −0.2102 | 0.034* | |
H6B | −0.0634 | 0.1493 | −0.2272 | 0.034* | |
C7 | 0.1743 (4) | 0.2356 (2) | −0.0763 (2) | 0.0220 (8) | |
C8 | 0.2892 (4) | 0.3042 (3) | −0.1090 (2) | 0.0308 (9) | |
H8A | 0.3748 | 0.2814 | −0.0953 | 0.037* | |
C9 | 0.2781 (4) | 0.4063 (3) | −0.1616 (3) | 0.0368 (10) | |
H9A | 0.3570 | 0.4529 | −0.1854 | 0.044* | |
C10 | 0.1528 (4) | 0.4404 (3) | −0.1796 (2) | 0.0373 (10) | |
H10A | 0.1454 | 0.5106 | −0.2144 | 0.045* | |
C11 | 0.0388 (4) | 0.3729 (3) | −0.1472 (2) | 0.0320 (9) | |
H11A | −0.0471 | 0.3966 | −0.1596 | 0.038* | |
C12 | 0.0493 (4) | 0.2698 (3) | −0.0964 (2) | 0.0240 (8) | |
H12A | −0.0289 | 0.2230 | −0.0754 | 0.029* | |
C13 | 0.2253 (3) | 0.1005 (3) | 0.0925 (2) | 0.0233 (8) | |
C14 | 0.2972 (4) | 0.0223 (3) | 0.1429 (2) | 0.0299 (9) | |
H14A | 0.3304 | −0.0294 | 0.1236 | 0.036* | |
C15 | 0.3197 (4) | 0.0204 (3) | 0.2210 (2) | 0.0347 (10) | |
H15A | 0.3700 | −0.0322 | 0.2546 | 0.042* | |
C16 | 0.2702 (4) | 0.0938 (3) | 0.2509 (3) | 0.0396 (10) | |
H16A | 0.2847 | 0.0908 | 0.3053 | 0.048* | |
C17 | 0.1997 (4) | 0.1716 (3) | 0.2014 (3) | 0.0399 (11) | |
H17A | 0.1657 | 0.2223 | 0.2218 | 0.048* | |
C18 | 0.1783 (4) | 0.1762 (3) | 0.1220 (2) | 0.0308 (9) | |
H18A | 0.1317 | 0.2308 | 0.0875 | 0.037* | |
C19 | 0.2724 (4) | −0.3735 (3) | −0.0693 (2) | 0.0261 (9) | |
C20 | 0.1804 (4) | −0.4595 (3) | −0.0227 (2) | 0.0340 (10) | |
H20A | 0.1102 | −0.4700 | −0.0487 | 0.041* | |
C21 | 0.1888 (5) | −0.5295 (3) | 0.0600 (3) | 0.0436 (11) | |
H21A | 0.1251 | −0.5875 | 0.0908 | 0.052* | |
C22 | 0.2916 (5) | −0.5138 (3) | 0.0973 (3) | 0.0495 (12) | |
H22A | 0.2984 | −0.5618 | 0.1543 | 0.059* | |
C23 | 0.3843 (5) | −0.4296 (3) | 0.0531 (3) | 0.0486 (12) | |
H23A | 0.4542 | −0.4199 | 0.0797 | 0.058* | |
C24 | 0.3753 (4) | −0.3594 (3) | −0.0300 (3) | 0.0369 (10) | |
H24A | 0.4392 | −0.3015 | −0.0605 | 0.044* | |
C25 | 0.3817 (4) | −0.2982 (2) | −0.2594 (2) | 0.0240 (8) | |
C26 | 0.3442 (4) | −0.3123 (3) | −0.3279 (2) | 0.0337 (10) | |
H26A | 0.2501 | −0.3134 | −0.3301 | 0.040* | |
C27 | 0.4446 (5) | −0.3247 (3) | −0.3938 (3) | 0.0440 (11) | |
H27A | 0.4181 | −0.3358 | −0.4399 | 0.053* | |
C28 | 0.5810 (5) | −0.3209 (3) | −0.3923 (3) | 0.0444 (11) | |
H28A | 0.6490 | −0.3287 | −0.4374 | 0.053* | |
C29 | 0.6188 (4) | −0.3057 (3) | −0.3250 (3) | 0.0452 (11) | |
H29A | 0.7132 | −0.3029 | −0.3239 | 0.054* | |
C30 | 0.5202 (4) | −0.2944 (3) | −0.2589 (3) | 0.0382 (10) | |
H30A | 0.5476 | −0.2840 | −0.2128 | 0.046* | |
C31 | 0.0423 (4) | 0.3607 (3) | −0.3693 (2) | 0.0321 (9) | |
C32 | 0.1357 (5) | 0.4441 (3) | −0.4216 (3) | 0.0454 (12) | |
H32A | 0.2227 | 0.4346 | −0.4524 | 0.054* | |
C33 | 0.1019 (6) | 0.5415 (3) | −0.4287 (3) | 0.0630 (15) | |
H33A | 0.1659 | 0.5984 | −0.4644 | 0.076* | |
C34 | −0.0245 (7) | 0.5558 (4) | −0.3839 (3) | 0.0664 (17) | |
H34A | −0.0467 | 0.6224 | −0.3885 | 0.080* | |
C35 | −0.1177 (5) | 0.4744 (3) | −0.3330 (3) | 0.0553 (14) | |
H35A | −0.2049 | 0.4850 | −0.3032 | 0.066* | |
C36 | −0.0856 (4) | 0.3765 (3) | −0.3245 (3) | 0.0426 (11) | |
H36A | −0.1503 | 0.3202 | −0.2883 | 0.051* | |
C37 | −0.0041 (4) | 0.1944 (3) | −0.4207 (2) | 0.0341 (10) | |
C38 | −0.1474 (5) | 0.1935 (3) | −0.4052 (3) | 0.0441 (11) | |
H38A | −0.1969 | 0.2136 | −0.3609 | 0.053* | |
C39 | −0.2181 (5) | 0.1636 (3) | −0.4537 (3) | 0.0600 (14) | |
H39A | −0.3155 | 0.1630 | −0.4424 | 0.072* | |
C40 | −0.1472 (7) | 0.1346 (4) | −0.5184 (4) | 0.0686 (16) | |
H40A | −0.1956 | 0.1146 | −0.5521 | 0.082* | |
C41 | −0.0054 (6) | 0.1346 (3) | −0.5342 (3) | 0.0628 (15) | |
H41A | 0.0434 | 0.1146 | −0.5788 | 0.075* | |
C42 | 0.0663 (5) | 0.1637 (3) | −0.4850 (3) | 0.0445 (11) | |
H42A | 0.1636 | 0.1625 | −0.4956 | 0.053* | |
C43 | 0.5176 (7) | 0.3611 (8) | −0.3513 (5) | 0.189 (5) | |
H43A | 0.4298 | 0.3719 | −0.3181 | 0.283* | |
H43B | 0.5889 | 0.4101 | −0.3563 | 0.283* | |
H43C | 0.5431 | 0.2914 | −0.3204 | 0.283* | |
O6 | 0.5062 (8) | 0.3739 (8) | −0.4264 (6) | 0.323 (5) | |
H6C | 0.4366 | 0.3392 | −0.4223 | 0.484* | |
O7 | 0.4255 (4) | 0.0828 (3) | −0.3559 (2) | 0.0696 (10) | |
H7A | 0.3781 | 0.1338 | −0.3694 | 0.104* | |
C44 | 0.4311 (5) | 0.0373 (4) | −0.4169 (3) | 0.0693 (15) | |
H44A | 0.4950 | −0.0172 | −0.4054 | 0.104* | |
H44B | 0.4629 | 0.0893 | −0.4772 | 0.104* | |
H44C | 0.3393 | 0.0086 | −0.4102 | 0.104* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.01772 (11) | 0.01445 (11) | 0.02003 (12) | 0.00337 (8) | −0.00161 (8) | −0.00841 (9) |
P1 | 0.0203 (5) | 0.0187 (5) | 0.0269 (5) | 0.0024 (4) | −0.0040 (4) | −0.0110 (4) |
P2 | 0.0212 (5) | 0.0184 (5) | 0.0226 (5) | 0.0036 (4) | −0.0014 (4) | −0.0094 (4) |
P3 | 0.0274 (6) | 0.0221 (5) | 0.0281 (6) | 0.0050 (4) | −0.0037 (5) | −0.0127 (5) |
P4 | 0.0335 (6) | 0.0252 (6) | 0.0243 (6) | 0.0036 (5) | −0.0035 (5) | −0.0067 (5) |
N1 | 0.024 (2) | 0.047 (2) | 0.050 (3) | −0.0001 (18) | −0.0083 (19) | −0.016 (2) |
O1 | 0.0253 (15) | 0.0367 (16) | 0.0403 (16) | 0.0043 (12) | −0.0074 (13) | −0.0177 (14) |
O2 | 0.0328 (16) | 0.0393 (17) | 0.0355 (16) | 0.0016 (13) | 0.0025 (13) | −0.0107 (14) |
O3 | 0.044 (2) | 0.175 (4) | 0.052 (2) | 0.013 (2) | −0.0171 (19) | 0.025 (3) |
O4 | 0.0298 (17) | 0.055 (2) | 0.065 (2) | 0.0065 (15) | −0.0073 (16) | −0.0283 (17) |
O5 | 0.0328 (17) | 0.0443 (18) | 0.0494 (19) | 0.0025 (14) | −0.0046 (15) | −0.0208 (16) |
C1 | 0.020 (2) | 0.0203 (19) | 0.035 (2) | 0.0030 (16) | −0.0052 (17) | −0.0121 (18) |
C2 | 0.022 (2) | 0.025 (2) | 0.032 (2) | 0.0009 (16) | 0.0017 (17) | −0.0147 (18) |
C3 | 0.028 (2) | 0.0185 (19) | 0.025 (2) | 0.0046 (16) | −0.0039 (17) | −0.0105 (17) |
C4 | 0.029 (2) | 0.0198 (19) | 0.032 (2) | 0.0054 (16) | −0.0019 (17) | −0.0122 (18) |
C5 | 0.028 (2) | 0.024 (2) | 0.021 (2) | 0.0027 (16) | −0.0019 (16) | −0.0094 (17) |
C6 | 0.031 (2) | 0.029 (2) | 0.026 (2) | 0.0117 (18) | −0.0061 (18) | −0.0121 (18) |
C7 | 0.025 (2) | 0.0199 (19) | 0.023 (2) | 0.0049 (16) | −0.0024 (16) | −0.0122 (16) |
C8 | 0.028 (2) | 0.026 (2) | 0.037 (2) | 0.0015 (18) | −0.0084 (19) | −0.0120 (19) |
C9 | 0.039 (3) | 0.024 (2) | 0.043 (3) | −0.0067 (19) | −0.007 (2) | −0.010 (2) |
C10 | 0.056 (3) | 0.019 (2) | 0.033 (2) | 0.007 (2) | −0.012 (2) | −0.0071 (19) |
C11 | 0.034 (2) | 0.031 (2) | 0.035 (2) | 0.0125 (19) | −0.0123 (19) | −0.016 (2) |
C12 | 0.023 (2) | 0.023 (2) | 0.025 (2) | 0.0022 (16) | −0.0035 (16) | −0.0107 (17) |
C13 | 0.019 (2) | 0.025 (2) | 0.026 (2) | −0.0022 (16) | −0.0032 (16) | −0.0118 (17) |
C14 | 0.028 (2) | 0.027 (2) | 0.034 (2) | 0.0050 (17) | −0.0048 (18) | −0.0131 (19) |
C15 | 0.029 (2) | 0.036 (2) | 0.034 (2) | 0.0038 (19) | −0.0110 (19) | −0.007 (2) |
C16 | 0.046 (3) | 0.045 (3) | 0.033 (2) | 0.000 (2) | −0.016 (2) | −0.017 (2) |
C17 | 0.053 (3) | 0.036 (2) | 0.042 (3) | 0.009 (2) | −0.018 (2) | −0.025 (2) |
C18 | 0.035 (2) | 0.028 (2) | 0.033 (2) | 0.0032 (18) | −0.0108 (19) | −0.0142 (19) |
C19 | 0.031 (2) | 0.022 (2) | 0.026 (2) | 0.0065 (17) | −0.0008 (17) | −0.0139 (18) |
C20 | 0.040 (3) | 0.028 (2) | 0.033 (2) | 0.0030 (19) | −0.002 (2) | −0.015 (2) |
C21 | 0.060 (3) | 0.024 (2) | 0.037 (3) | 0.005 (2) | 0.001 (2) | −0.010 (2) |
C22 | 0.068 (3) | 0.035 (3) | 0.037 (3) | 0.024 (2) | −0.013 (3) | −0.005 (2) |
C23 | 0.053 (3) | 0.053 (3) | 0.046 (3) | 0.015 (3) | −0.023 (2) | −0.021 (3) |
C24 | 0.039 (3) | 0.034 (2) | 0.038 (3) | 0.005 (2) | −0.009 (2) | −0.014 (2) |
C25 | 0.030 (2) | 0.0147 (18) | 0.024 (2) | 0.0037 (16) | −0.0013 (17) | −0.0070 (16) |
C26 | 0.038 (3) | 0.032 (2) | 0.032 (2) | 0.0015 (19) | −0.007 (2) | −0.014 (2) |
C27 | 0.055 (3) | 0.051 (3) | 0.030 (2) | 0.000 (2) | −0.004 (2) | −0.022 (2) |
C28 | 0.049 (3) | 0.045 (3) | 0.031 (3) | 0.004 (2) | 0.010 (2) | −0.018 (2) |
C29 | 0.034 (3) | 0.057 (3) | 0.042 (3) | 0.011 (2) | 0.000 (2) | −0.022 (2) |
C30 | 0.037 (3) | 0.047 (3) | 0.033 (2) | 0.008 (2) | −0.004 (2) | −0.021 (2) |
C31 | 0.045 (3) | 0.025 (2) | 0.025 (2) | 0.0034 (19) | −0.012 (2) | −0.0065 (18) |
C32 | 0.066 (3) | 0.033 (3) | 0.035 (3) | −0.001 (2) | −0.020 (2) | −0.007 (2) |
C33 | 0.109 (5) | 0.027 (3) | 0.048 (3) | −0.006 (3) | −0.032 (3) | −0.002 (2) |
C34 | 0.128 (5) | 0.028 (3) | 0.057 (4) | 0.026 (3) | −0.049 (4) | −0.017 (3) |
C35 | 0.087 (4) | 0.042 (3) | 0.052 (3) | 0.034 (3) | −0.037 (3) | −0.025 (3) |
C36 | 0.058 (3) | 0.030 (2) | 0.042 (3) | 0.014 (2) | −0.021 (2) | −0.013 (2) |
C37 | 0.048 (3) | 0.022 (2) | 0.027 (2) | 0.0042 (19) | −0.009 (2) | −0.0047 (18) |
C38 | 0.052 (3) | 0.037 (3) | 0.040 (3) | 0.000 (2) | −0.014 (2) | −0.010 (2) |
C39 | 0.069 (4) | 0.046 (3) | 0.065 (4) | −0.001 (3) | −0.033 (3) | −0.012 (3) |
C40 | 0.099 (5) | 0.045 (3) | 0.066 (4) | −0.010 (3) | −0.046 (4) | −0.012 (3) |
C41 | 0.109 (5) | 0.042 (3) | 0.042 (3) | 0.002 (3) | −0.023 (3) | −0.019 (3) |
C42 | 0.066 (3) | 0.031 (2) | 0.038 (3) | 0.004 (2) | −0.016 (2) | −0.013 (2) |
C43 | 0.124 (7) | 0.398 (14) | 0.106 (6) | −0.101 (8) | 0.031 (5) | −0.185 (8) |
O6 | 0.201 (7) | 0.614 (17) | 0.306 (11) | 0.094 (10) | −0.050 (7) | −0.350 (12) |
O7 | 0.069 (3) | 0.088 (3) | 0.056 (2) | 0.026 (2) | −0.0123 (19) | −0.036 (2) |
C44 | 0.095 (4) | 0.066 (4) | 0.050 (3) | 0.001 (3) | −0.009 (3) | −0.031 (3) |
Pt1—P2i | 2.3235 (9) | C17—H17A | 0.9500 |
Pt1—P2 | 2.3236 (9) | C18—H18A | 0.9500 |
Pt1—P1i | 2.3399 (9) | C19—C20 | 1.396 (5) |
Pt1—P1 | 2.3399 (9) | C19—C24 | 1.400 (5) |
Pt1—O4 | 3.524 (3) | C20—C21 | 1.377 (5) |
P1—C7 | 1.818 (3) | C20—H20A | 0.9500 |
P1—C13 | 1.823 (3) | C21—C22 | 1.385 (6) |
P1—C1 | 1.825 (3) | C21—H21A | 0.9500 |
P2—C3 | 1.826 (3) | C22—C23 | 1.380 (6) |
P2—C5 | 1.828 (3) | C22—H22A | 0.9500 |
P2—C2 | 1.838 (3) | C23—C24 | 1.386 (5) |
P3—O1 | 1.492 (2) | C23—H23A | 0.9500 |
P3—C19 | 1.801 (4) | C24—H24A | 0.9500 |
P3—C25 | 1.808 (3) | C25—C26 | 1.384 (5) |
P3—C4 | 1.814 (3) | C25—C30 | 1.388 (5) |
P4—O2 | 1.494 (3) | C26—C27 | 1.399 (5) |
P4—C31 | 1.796 (4) | C26—H26A | 0.9500 |
P4—C6 | 1.801 (3) | C27—C28 | 1.372 (5) |
P4—C37 | 1.804 (4) | C27—H27A | 0.9500 |
N1—O3 | 1.228 (4) | C28—C29 | 1.373 (5) |
N1—O4 | 1.242 (4) | C28—H28A | 0.9500 |
N1—O5 | 1.247 (4) | C29—C30 | 1.384 (5) |
C1—C2 | 1.529 (4) | C29—H29A | 0.9500 |
C1—H1B | 0.9900 | C30—H30A | 0.9500 |
C1—H1C | 0.9900 | C31—C32 | 1.390 (5) |
C2—H2B | 0.9900 | C31—C36 | 1.403 (5) |
C2—H2C | 0.9900 | C32—C33 | 1.390 (6) |
C3—C4 | 1.545 (4) | C32—H32A | 0.9500 |
C3—H3A | 0.9900 | C33—C34 | 1.382 (7) |
C3—H3B | 0.9900 | C33—H33A | 0.9500 |
C4—H4A | 0.9900 | C34—C35 | 1.367 (6) |
C4—H4B | 0.9900 | C34—H34A | 0.9500 |
C5—C6 | 1.543 (4) | C35—C36 | 1.388 (5) |
C5—H5A | 0.9900 | C35—H35A | 0.9500 |
C5—H5B | 0.9900 | C36—H36A | 0.9500 |
C6—H6A | 0.9900 | C37—C42 | 1.386 (5) |
C6—H6B | 0.9900 | C37—C38 | 1.398 (5) |
C7—C12 | 1.391 (4) | C38—C39 | 1.384 (6) |
C7—C8 | 1.391 (5) | C38—H38A | 0.9500 |
C8—C9 | 1.390 (5) | C39—C40 | 1.378 (7) |
C8—H8A | 0.9500 | C39—H39A | 0.9500 |
C9—C10 | 1.383 (5) | C40—C41 | 1.383 (7) |
C9—H9A | 0.9500 | C40—H40A | 0.9500 |
C10—C11 | 1.376 (5) | C41—C42 | 1.394 (6) |
C10—H10A | 0.9500 | C41—H41A | 0.9500 |
C11—C12 | 1.393 (5) | C42—H42A | 0.9500 |
C11—H11A | 0.9500 | C43—O6 | 1.244 (8) |
C12—H12A | 0.9500 | C43—H43A | 0.9800 |
C13—C14 | 1.398 (5) | C43—H43B | 0.9800 |
C13—C18 | 1.399 (5) | C43—H43C | 0.9800 |
C14—C15 | 1.383 (5) | O6—H6C | 0.8400 |
C14—H14A | 0.9500 | O7—C44 | 1.422 (5) |
C15—C16 | 1.380 (5) | O7—H7A | 0.8400 |
C15—H15A | 0.9500 | C44—H44A | 0.9800 |
C16—C17 | 1.381 (5) | C44—H44B | 0.9800 |
C16—H16A | 0.9500 | C44—H44C | 0.9800 |
C17—C18 | 1.387 (5) | ||
P2i—Pt1—P2 | 180.0 | C16—C15—C14 | 121.0 (4) |
P2i—Pt1—P1i | 83.40 (3) | C16—C15—H15A | 119.5 |
P2—Pt1—P1i | 96.60 (3) | C14—C15—H15A | 119.5 |
P2i—Pt1—P1 | 96.60 (3) | C15—C16—C17 | 119.7 (4) |
P2—Pt1—P1 | 83.40 (3) | C15—C16—H16A | 120.2 |
P1i—Pt1—P1 | 180.0 | C17—C16—H16A | 120.2 |
P2i—Pt1—O4 | 80.23 (5) | C16—C17—C18 | 120.3 (4) |
P2—Pt1—O4 | 99.77 (5) | C16—C17—H17A | 119.8 |
P1i—Pt1—O4 | 75.64 (5) | C18—C17—H17A | 119.8 |
P1—Pt1—O4 | 104.36 (5) | C17—C18—C13 | 120.2 (3) |
C7—P1—C13 | 104.93 (16) | C17—C18—H18A | 119.9 |
C7—P1—C1 | 105.46 (16) | C13—C18—H18A | 119.9 |
C13—P1—C1 | 107.00 (16) | C20—C19—C24 | 118.4 (3) |
C7—P1—Pt1 | 111.66 (12) | C20—C19—P3 | 118.1 (3) |
C13—P1—Pt1 | 120.67 (11) | C24—C19—P3 | 123.5 (3) |
C1—P1—Pt1 | 106.12 (11) | C21—C20—C19 | 121.7 (4) |
C3—P2—C5 | 106.78 (15) | C21—C20—H20A | 119.2 |
C3—P2—C2 | 106.38 (16) | C19—C20—H20A | 119.2 |
C5—P2—C2 | 104.19 (16) | C20—C21—C22 | 118.9 (4) |
C3—P2—Pt1 | 112.39 (11) | C20—C21—H21A | 120.6 |
C5—P2—Pt1 | 117.14 (11) | C22—C21—H21A | 120.6 |
C2—P2—Pt1 | 109.17 (11) | C23—C22—C21 | 121.0 (4) |
O1—P3—C19 | 112.39 (16) | C23—C22—H22A | 119.5 |
O1—P3—C25 | 112.26 (16) | C21—C22—H22A | 119.5 |
C19—P3—C25 | 107.85 (16) | C22—C23—C24 | 119.9 (4) |
O1—P3—C4 | 111.99 (16) | C22—C23—H23A | 120.1 |
C19—P3—C4 | 106.38 (16) | C24—C23—H23A | 120.1 |
C25—P3—C4 | 105.54 (16) | C23—C24—C19 | 120.2 (4) |
O2—P4—C31 | 112.08 (17) | C23—C24—H24A | 119.9 |
O2—P4—C6 | 111.78 (16) | C19—C24—H24A | 119.9 |
C31—P4—C6 | 106.10 (17) | C26—C25—C30 | 118.7 (3) |
O2—P4—C37 | 110.24 (17) | C26—C25—P3 | 118.5 (3) |
C31—P4—C37 | 108.83 (17) | C30—C25—P3 | 122.8 (3) |
C6—P4—C37 | 107.61 (17) | C25—C26—C27 | 120.2 (4) |
O3—N1—O4 | 118.8 (4) | C25—C26—H26A | 119.9 |
O3—N1—O5 | 121.3 (4) | C27—C26—H26A | 119.9 |
O4—N1—O5 | 119.8 (4) | C28—C27—C26 | 120.4 (4) |
N1—O4—Pt1 | 148.3 (3) | C28—C27—H27A | 119.8 |
C2—C1—P1 | 108.3 (2) | C26—C27—H27A | 119.8 |
C2—C1—H1B | 110.0 | C27—C28—C29 | 119.6 (4) |
P1—C1—H1B | 110.0 | C27—C28—H28A | 120.2 |
C2—C1—H1C | 110.0 | C29—C28—H28A | 120.2 |
P1—C1—H1C | 110.0 | C28—C29—C30 | 120.5 (4) |
H1B—C1—H1C | 108.4 | C28—C29—H29A | 119.8 |
C1—C2—P2 | 110.6 (2) | C30—C29—H29A | 119.8 |
C1—C2—H2B | 109.5 | C29—C30—C25 | 120.7 (4) |
P2—C2—H2B | 109.5 | C29—C30—H30A | 119.7 |
C1—C2—H2C | 109.5 | C25—C30—H30A | 119.7 |
P2—C2—H2C | 109.5 | C32—C31—C36 | 119.1 (4) |
H2B—C2—H2C | 108.1 | C32—C31—P4 | 118.4 (3) |
C4—C3—P2 | 116.6 (2) | C36—C31—P4 | 122.5 (3) |
C4—C3—H3A | 108.1 | C31—C32—C33 | 120.0 (5) |
P2—C3—H3A | 108.1 | C31—C32—H32A | 120.0 |
C4—C3—H3B | 108.1 | C33—C32—H32A | 120.0 |
P2—C3—H3B | 108.1 | C34—C33—C32 | 120.3 (5) |
H3A—C3—H3B | 107.3 | C34—C33—H33A | 119.9 |
C3—C4—P3 | 109.4 (2) | C32—C33—H33A | 119.9 |
C3—C4—H4A | 109.8 | C35—C34—C33 | 120.2 (5) |
P3—C4—H4A | 109.8 | C35—C34—H34A | 119.9 |
C3—C4—H4B | 109.8 | C33—C34—H34A | 119.9 |
P3—C4—H4B | 109.8 | C34—C35—C36 | 120.4 (5) |
H4A—C4—H4B | 108.3 | C34—C35—H35A | 119.8 |
C6—C5—P2 | 111.1 (2) | C36—C35—H35A | 119.8 |
C6—C5—H5A | 109.4 | C35—C36—C31 | 120.0 (4) |
P2—C5—H5A | 109.4 | C35—C36—H36A | 120.0 |
C6—C5—H5B | 109.4 | C31—C36—H36A | 120.0 |
P2—C5—H5B | 109.4 | C42—C37—C38 | 118.8 (4) |
H5A—C5—H5B | 108.0 | C42—C37—P4 | 119.2 (3) |
C5—C6—P4 | 112.2 (2) | C38—C37—P4 | 122.0 (3) |
C5—C6—H6A | 109.2 | C39—C38—C37 | 120.9 (4) |
P4—C6—H6A | 109.2 | C39—C38—H38A | 119.6 |
C5—C6—H6B | 109.2 | C37—C38—H38A | 119.6 |
P4—C6—H6B | 109.2 | C40—C39—C38 | 120.0 (5) |
H6A—C6—H6B | 107.9 | C40—C39—H39A | 120.0 |
C12—C7—C8 | 119.7 (3) | C38—C39—H39A | 120.0 |
C12—C7—P1 | 119.6 (3) | C39—C40—C41 | 119.8 (5) |
C8—C7—P1 | 120.7 (3) | C39—C40—H40A | 120.1 |
C9—C8—C7 | 119.7 (3) | C41—C40—H40A | 120.1 |
C9—C8—H8A | 120.1 | C40—C41—C42 | 120.5 (5) |
C7—C8—H8A | 120.1 | C40—C41—H41A | 119.8 |
C10—C9—C8 | 120.3 (4) | C42—C41—H41A | 119.8 |
C10—C9—H9A | 119.8 | C37—C42—C41 | 120.1 (4) |
C8—C9—H9A | 119.8 | C37—C42—H42A | 120.0 |
C11—C10—C9 | 120.2 (4) | C41—C42—H42A | 120.0 |
C11—C10—H10A | 119.9 | O6—C43—H43A | 109.5 |
C9—C10—H10A | 119.9 | O6—C43—H43B | 109.5 |
C10—C11—C12 | 120.1 (3) | H43A—C43—H43B | 109.5 |
C10—C11—H11A | 119.9 | O6—C43—H43C | 109.5 |
C12—C11—H11A | 119.9 | H43A—C43—H43C | 109.5 |
C7—C12—C11 | 119.9 (3) | H43B—C43—H43C | 109.5 |
C7—C12—H12A | 120.0 | C43—O6—H6C | 109.5 |
C11—C12—H12A | 120.0 | C44—O7—H7A | 109.5 |
C14—C13—C18 | 119.1 (3) | O7—C44—H44A | 109.5 |
C14—C13—P1 | 120.8 (3) | O7—C44—H44B | 109.5 |
C18—C13—P1 | 120.0 (3) | H44A—C44—H44B | 109.5 |
C15—C14—C13 | 119.7 (3) | O7—C44—H44C | 109.5 |
C15—C14—H14A | 120.1 | H44A—C44—H44C | 109.5 |
C13—C14—H14A | 120.1 | H44B—C44—H44C | 109.5 |
Symmetry code: (i) −x, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6C···O2 | 0.84 | 2.32 | 3.160 (9) | 174 |
O7—H7A···O2 | 0.84 | 1.95 | 2.777 (4) | 170 |
C12—H12A···O4 | 0.95 | 2.29 | 3.132 (4) | 147 |
C6—H6B···O4 | 0.99 | 2.53 | 3.294 (4) | 134 |
C1—H1B···O5ii | 0.99 | 2.42 | 3.289 (5) | 146 |
C1—H1C···O5i | 0.99 | 2.44 | 3.399 (5) | 162 |
C8—H8A···O3ii | 0.95 | 2.58 | 3.376 (5) | 142 |
C14—H14A···O4i | 0.95 | 2.56 | 3.317 (5) | 137 |
C27—H27A···O6iii | 0.95 | 2.50 | 3.338 (11) | 147 |
C28—H28A···O2iii | 0.95 | 2.60 | 3.385 (5) | 141 |
Symmetry codes: (i) −x, −y, −z; (ii) x+1, y, z; (iii) −x+1, −y, −z−1. |
Experimental details
Crystal data | |
Chemical formula | [Pt(NO3)2(C42H42O2P4)2]·4CH4O |
Mr | 1852.64 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 153 |
a, b, c (Å) | 9.9905 (9), 14.3346 (13), 16.9916 (15) |
α, β, γ (°) | 66.200 (1), 77.479 (1), 88.477 (1) |
V (Å3) | 2168.4 (3) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.83 |
Crystal size (mm) | 0.48 × 0.10 × 0.03 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1995) |
Tmin, Tmax | 0.474, 0.947 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 25181, 9347, 8160 |
Rint | 0.052 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.068, 0.91 |
No. of reflections | 9347 |
No. of parameters | 512 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.31, −1.37 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Pt1—P2 | 2.3236 (9) | Pt1—O4 | 3.524 (3) |
Pt1—P1 | 2.3399 (9) | ||
P2—Pt1—P1 | 83.40 (3) | P1—Pt1—O4 | 104.36 (5) |
P2—Pt1—O4 | 99.77 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6C···O2 | 0.84 | 2.32 | 3.160 (9) | 174 |
O7—H7A···O2 | 0.84 | 1.95 | 2.777 (4) | 170 |
C12—H12A···O4 | 0.95 | 2.29 | 3.132 (4) | 147 |
C6—H6B···O4 | 0.99 | 2.53 | 3.294 (4) | 134 |
C1—H1B···O5i | 0.99 | 2.42 | 3.289 (5) | 146 |
C1—H1C···O5ii | 0.99 | 2.44 | 3.399 (5) | 162 |
C8—H8A···O3i | 0.95 | 2.58 | 3.376 (5) | 142 |
C14—H14A···O4ii | 0.95 | 2.56 | 3.317 (5) | 137 |
C27—H27A···O6iii | 0.95 | 2.50 | 3.338 (11) | 147 |
C28—H28A···O2iii | 0.95 | 2.60 | 3.385 (5) | 141 |
Symmetry codes: (i) x+1, y, z; (ii) −x, −y, −z; (iii) −x+1, −y, −z−1. |
The title compound, [Pt(L)2]2+ (NO3-)2 (L = (P1,P1-bis(2-(diphenylphosphinoxid)ethyl)-P2,P2-diphenylethane -1,2-diphosphine), crystallizes as a packing of a discrete dication and two nitrate anions with the Pt-atom positioned on a centre of inversion. The two symmetry equivalent ligands molecules L are coordinated to the Pt-center by two phosphine donor atoms P1 and P2 with Pt—P distances (d(Pt—P1) = 2.3399 (9) Å, d(Pt—P2) = 2.3236 (9) Å) (Table 1) creating a square planar coordination environment in accord with previously reported PtII tetraphosphine complexes (Brüggeller et al., 1992). The two additional phosphor oxide groups of the ligands are not coordinated to the metal centre in the solid state. A long distance of d(Pt1—O4) = 3.524 (3) Å, angles of P1—Pt—O4 of 104.36 (5) ° and P2—Pt—O4 of 99.77 (5) ° are indicative of a weak Pt—NO3- interaction which is much weaker than a previously reported PtII—NO3- distance of 2.116 Å in a related complex (Fernandez et al., 2001). The nitrate anion is packed within a cavity created by the coordinated phosphine ligand atoms above and due to symmetry below the square plane spanned by the four phosphor ligand atoms creating a distorted octahedral coordination environment around the PtII ion. In addition several close C—H···O contacts between 2.30 and 2.70 Å were found between ortho-phenyl protons and methylene protons with nitrate oxygen atoms. Two methanol molecules with O—H···O hydrogen bonds to one of the O—P groups (Table 2) complete the crystal packing. The second P—O1 fragment exhibits weak hydrogen bond interactions with d(O1—H17A) of 2.997 Å and d(O1—H18A) of 2.991 Å to one of the adjacent phenyl group hydrogen atoms.