Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807029200/ng2281sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807029200/ng2281Isup2.hkl |
CCDC reference: 654796
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.006 Å
- R factor = 0.029
- wR factor = 0.072
- Data-to-parameter ratio = 18.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.35 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 12 CL2 -PT1 -P2 -C21 157.70 0.40 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 15 CL2 -PT1 -P2 -C15 -76.90 0.50 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 18 CL2 -PT1 -P2 -C27 38.10 0.50 1.555 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For the related cis-dichlorobis(methyldiphenylphosphine)platinum, see Ho et al. (1982).
For related literature, see: Domańska-Babul, Chojnacki, Matern & Pikies (2007); Krautscheid et al. (1997); Porzio et al. (1980).
The compound was been obtained as yellow powder by the reaction of a solution of ethyl(diphenyl)phosphane in ethanol with a solution of potassium tetrachloroplatinate(II) in water. It was obtained in a crystalline habit from the reaction of (iPr2N)2P–P(SiMe3)2 with [(EtPh2P)2PtCl2] a 1:1 molar ratio in THF. Crystals were obtained by recrystallization from pentane at 249 K
All C–H hydrogen atoms were refined as riding on carbon atoms with methyl C–H = 0.98 Å, methylen C–H = 0.99 Å, aromatic C–H = 0.95 Å and Uiso(H)=1.2 Ueq(C) for aromatic CH, 1.3 for CH2 groups and 1.5 for methyl groups.
In the course of our studies upon the reactivity of [(R3P)2MCl2] towards R'2P–P(SiMe3)2 (Domańska-Babul et al., 2007) we have studied the reaction of (iPr2N)2P–P(SiMe3)2 with [(EtPh2P)2PtCl2]. The title compound was obtained unchanged in the synthesis.
The complex exhibits square-planar coordination that is typical for platinum(II) compounds. The platinum atom is 0.0556 (4) Å above the square plane. The structure is similar to that of [(MePh2P)2PtCl2] (Ho et al., 1982). The square planar geometry is characteristic of complexes having less bulky tertiary phosphines. Significant deviation from planarity is observed with sterically bulky phosphines ligands, as noted in cis-dichlorobis(di-t-butylphenylphosphine)platinum(II) (Krautscheid et al., 1997; Porzio et al., 1980). The bond dimensions involving the platinum atom are typical of [cis-(R3P)2PtCl2] compounds such as for [(MePh2P)2PtCl2]. Weak intermolecular C—H···Cl interactions are also present.
For the related cis-dichlorobis(methyldiphenylphosphine)platinum, see Ho et al. (1982).
For related literature, see: Domańska-Babul, Chojnacki, Matern & Pikies (2007); Krautscheid et al. (1997); Porzio et al. (1980).
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999) and PLATON (Spek, 2003).
[PtCl2(C14H15P)2] | F(000) = 1360 |
Mr = 694.45 | Dx = 1.791 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9761 reflections |
a = 14.2831 (6) Å | θ = 2.9–32.5° |
b = 11.1025 (5) Å | µ = 5.80 mm−1 |
c = 16.9556 (7) Å | T = 120 K |
β = 106.677 (4)° | Prism, yellow |
V = 2575.69 (19) Å3 | 0.26 × 0.14 × 0.07 mm |
Z = 4 |
Oxford Diffraction KM-4-CCD diffractometer | 5413 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
0.75° ω scans | θmax = 27°, θmin = 2.9° |
Absorption correction: analytical CrysAlis RED (Oxford Diffraction, 2006; Clark & Reid, 1995). | h = −18→18 |
Tmin = 0.232, Tmax = 0.501 | k = −14→14 |
19512 measured reflections | l = −21→13 |
5614 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.029 | w = 1/[σ2(Fo2) + (0.0399P)2 + 6.0673P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.072 | (Δ/σ)max = 0.001 |
S = 1.10 | Δρmax = 2.88 e Å−3 |
5614 reflections | Δρmin = −1.23 e Å−3 |
300 parameters |
[PtCl2(C14H15P)2] | V = 2575.69 (19) Å3 |
Mr = 694.45 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 14.2831 (6) Å | µ = 5.80 mm−1 |
b = 11.1025 (5) Å | T = 120 K |
c = 16.9556 (7) Å | 0.26 × 0.14 × 0.07 mm |
β = 106.677 (4)° |
Oxford Diffraction KM-4-CCD diffractometer | 5614 independent reflections |
Absorption correction: analytical CrysAlis RED (Oxford Diffraction, 2006; Clark & Reid, 1995). | 5413 reflections with I > 2σ(I) |
Tmin = 0.232, Tmax = 0.501 | Rint = 0.032 |
19512 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.072 | H-atom parameters constrained |
S = 1.10 | Δρmax = 2.88 e Å−3 |
5614 reflections | Δρmin = −1.23 e Å−3 |
300 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. |
x | y | z | Uiso*/Ueq | ||
Pt1 | 0.270906 (9) | 0.459023 (11) | 0.282544 (7) | 0.01446 (6) | |
P1 | 0.15530 (6) | 0.41497 (8) | 0.34561 (5) | 0.01523 (17) | |
P2 | 0.36679 (6) | 0.29500 (8) | 0.31639 (5) | 0.01523 (17) | |
Cl1 | 0.36472 (8) | 0.53298 (8) | 0.20004 (6) | 0.0278 (2) | |
Cl2 | 0.17113 (7) | 0.62945 (9) | 0.23685 (6) | 0.0308 (2) | |
C1 | 0.1445 (3) | 0.5374 (3) | 0.4142 (2) | 0.0167 (7) | |
C2 | 0.0551 (3) | 0.5606 (3) | 0.4295 (2) | 0.0221 (7) | |
H2 | −0.0001 | 0.5119 | 0.4043 | 0.027* | |
C3 | 0.0462 (3) | 0.6541 (3) | 0.4811 (2) | 0.0256 (8) | |
H3 | −0.0152 | 0.6699 | 0.4904 | 0.031* | |
C4 | 0.1265 (3) | 0.7245 (3) | 0.5193 (2) | 0.0268 (8) | |
H4 | 0.1207 | 0.7873 | 0.5557 | 0.032* | |
C5 | 0.2154 (3) | 0.7028 (4) | 0.5043 (2) | 0.0287 (8) | |
H5 | 0.2705 | 0.7513 | 0.5301 | 0.034* | |
C6 | 0.2243 (3) | 0.6101 (3) | 0.4515 (2) | 0.0244 (8) | |
H6 | 0.2852 | 0.5964 | 0.441 | 0.029* | |
C7 | 0.1573 (3) | 0.2795 (3) | 0.4077 (2) | 0.0179 (7) | |
C8 | 0.0867 (3) | 0.1887 (3) | 0.3837 (2) | 0.0258 (8) | |
H8 | 0.0362 | 0.1962 | 0.3333 | 0.031* | |
C9 | 0.0898 (4) | 0.0879 (4) | 0.4328 (3) | 0.0357 (10) | |
H9 | 0.0402 | 0.0284 | 0.4168 | 0.043* | |
C10 | 0.1648 (4) | 0.0736 (4) | 0.5049 (3) | 0.0386 (11) | |
H10 | 0.1679 | 0.0031 | 0.5373 | 0.046* | |
C11 | 0.2353 (4) | 0.1624 (4) | 0.5297 (2) | 0.0316 (9) | |
H11 | 0.2874 | 0.1524 | 0.5788 | 0.038* | |
C12 | 0.2297 (3) | 0.2667 (3) | 0.4825 (2) | 0.0227 (7) | |
H12 | 0.2758 | 0.3296 | 0.5016 | 0.027* | |
C13 | 0.0365 (3) | 0.4052 (4) | 0.2677 (2) | 0.0225 (7) | |
H13A | −0.0121 | 0.3729 | 0.2937 | 0.029* | |
H13B | 0.0152 | 0.4873 | 0.2475 | 0.029* | |
C14 | 0.0376 (3) | 0.3256 (4) | 0.1944 (2) | 0.0300 (9) | |
H14A | 0.0771 | 0.3641 | 0.1629 | 0.045* | |
H14B | −0.0294 | 0.3148 | 0.159 | 0.045* | |
H14C | 0.0657 | 0.247 | 0.2144 | 0.045* | |
C15 | 0.2996 (3) | 0.1563 (3) | 0.2819 (2) | 0.0181 (7) | |
C16 | 0.2805 (3) | 0.0686 (3) | 0.3338 (2) | 0.0212 (7) | |
H16 | 0.2992 | 0.0818 | 0.3916 | 0.025* | |
C17 | 0.2339 (3) | −0.0384 (3) | 0.3015 (3) | 0.0237 (8) | |
H17 | 0.2212 | −0.098 | 0.3373 | 0.028* | |
C18 | 0.2061 (3) | −0.0577 (4) | 0.2169 (3) | 0.0249 (8) | |
H18 | 0.1767 | −0.1319 | 0.1951 | 0.03* | |
C19 | 0.2210 (3) | 0.0305 (4) | 0.1648 (3) | 0.0298 (9) | |
H19 | 0.1994 | 0.0187 | 0.1069 | 0.036* | |
C20 | 0.2678 (3) | 0.1370 (4) | 0.1970 (2) | 0.0280 (8) | |
H20 | 0.2782 | 0.1974 | 0.1607 | 0.034* | |
C21 | 0.4359 (2) | 0.2718 (3) | 0.4232 (2) | 0.0184 (7) | |
C22 | 0.4926 (3) | 0.1674 (4) | 0.4455 (3) | 0.0284 (8) | |
H22 | 0.4899 | 0.1057 | 0.4061 | 0.034* | |
C23 | 0.5528 (3) | 0.1547 (4) | 0.5254 (3) | 0.0332 (9) | |
H23 | 0.5913 | 0.0839 | 0.5402 | 0.04* | |
C24 | 0.5576 (3) | 0.2429 (4) | 0.5837 (2) | 0.0333 (10) | |
H24 | 0.5987 | 0.2325 | 0.6383 | 0.04* | |
C25 | 0.5021 (3) | 0.3470 (4) | 0.5622 (2) | 0.0295 (9) | |
H25 | 0.5046 | 0.4077 | 0.6023 | 0.035* | |
C26 | 0.4427 (3) | 0.3623 (3) | 0.4817 (2) | 0.0225 (7) | |
H26 | 0.4066 | 0.4348 | 0.4666 | 0.027* | |
C27 | 0.4649 (3) | 0.2823 (4) | 0.2668 (2) | 0.0232 (7) | |
H27A | 0.4863 | 0.1972 | 0.2697 | 0.03* | |
H27B | 0.4379 | 0.3034 | 0.2079 | 0.03* | |
C28 | 0.5551 (3) | 0.3615 (4) | 0.3040 (3) | 0.0313 (9) | |
H28A | 0.5372 | 0.4465 | 0.2938 | 0.047* | |
H28B | 0.6065 | 0.3414 | 0.2783 | 0.047* | |
H28C | 0.5791 | 0.3472 | 0.3634 | 0.047* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.01654 (8) | 0.01163 (8) | 0.01519 (8) | −0.00052 (4) | 0.00450 (5) | 0.00112 (4) |
P1 | 0.0155 (4) | 0.0138 (4) | 0.0161 (4) | 0.0003 (3) | 0.0041 (3) | −0.0004 (3) |
P2 | 0.0140 (4) | 0.0137 (4) | 0.0174 (4) | −0.0005 (3) | 0.0037 (3) | −0.0013 (3) |
Cl1 | 0.0330 (5) | 0.0240 (5) | 0.0315 (5) | −0.0059 (4) | 0.0174 (4) | 0.0040 (3) |
Cl2 | 0.0351 (5) | 0.0213 (4) | 0.0369 (5) | 0.0105 (4) | 0.0121 (4) | 0.0129 (4) |
C1 | 0.0216 (17) | 0.0132 (16) | 0.0164 (16) | 0.0034 (12) | 0.0072 (14) | 0.0024 (12) |
C2 | 0.0253 (19) | 0.0192 (17) | 0.0244 (18) | −0.0008 (14) | 0.0111 (15) | 0.0020 (14) |
C3 | 0.034 (2) | 0.0206 (18) | 0.0275 (19) | 0.0058 (15) | 0.0176 (16) | 0.0023 (15) |
C4 | 0.045 (2) | 0.0164 (17) | 0.0201 (17) | 0.0039 (16) | 0.0118 (16) | −0.0002 (14) |
C5 | 0.033 (2) | 0.0226 (19) | 0.027 (2) | −0.0041 (16) | 0.0029 (16) | −0.0045 (16) |
C6 | 0.0220 (18) | 0.0225 (18) | 0.0272 (18) | 0.0005 (14) | 0.0045 (15) | −0.0034 (15) |
C7 | 0.0203 (16) | 0.0157 (16) | 0.0198 (16) | −0.0002 (13) | 0.0090 (13) | −0.0010 (13) |
C8 | 0.0266 (19) | 0.0230 (19) | 0.030 (2) | −0.0086 (15) | 0.0116 (16) | −0.0073 (15) |
C9 | 0.051 (3) | 0.024 (2) | 0.040 (2) | −0.0164 (19) | 0.024 (2) | −0.0079 (18) |
C10 | 0.074 (3) | 0.0173 (19) | 0.032 (2) | −0.006 (2) | 0.028 (2) | 0.0026 (17) |
C11 | 0.052 (3) | 0.0221 (19) | 0.0204 (18) | 0.0032 (18) | 0.0101 (17) | −0.0003 (15) |
C12 | 0.0294 (19) | 0.0163 (17) | 0.0228 (17) | 0.0001 (14) | 0.0081 (15) | −0.0020 (14) |
C13 | 0.0164 (16) | 0.0253 (19) | 0.0225 (17) | 0.0018 (14) | 0.0003 (13) | −0.0030 (14) |
C14 | 0.0258 (19) | 0.036 (2) | 0.0238 (19) | 0.0035 (17) | −0.0006 (15) | −0.0048 (17) |
C15 | 0.0174 (16) | 0.0125 (16) | 0.0232 (17) | 0.0018 (13) | 0.0036 (13) | −0.0027 (13) |
C16 | 0.0215 (17) | 0.0209 (17) | 0.0210 (17) | 0.0003 (14) | 0.0060 (14) | −0.0007 (14) |
C17 | 0.0224 (19) | 0.0180 (18) | 0.032 (2) | −0.0005 (13) | 0.0097 (16) | 0.0003 (14) |
C18 | 0.0199 (17) | 0.0193 (18) | 0.034 (2) | −0.0024 (14) | 0.0058 (15) | −0.0071 (15) |
C19 | 0.033 (2) | 0.028 (2) | 0.025 (2) | −0.0058 (16) | 0.0031 (17) | −0.0062 (16) |
C20 | 0.038 (2) | 0.0209 (19) | 0.0211 (18) | −0.0082 (16) | 0.0017 (16) | 0.0010 (15) |
C21 | 0.0155 (15) | 0.0182 (17) | 0.0182 (16) | −0.0031 (13) | −0.0006 (12) | −0.0014 (13) |
C22 | 0.0238 (19) | 0.0234 (19) | 0.034 (2) | 0.0019 (15) | 0.0019 (16) | 0.0030 (16) |
C23 | 0.025 (2) | 0.030 (2) | 0.038 (2) | 0.0001 (16) | −0.0030 (17) | 0.0126 (18) |
C24 | 0.028 (2) | 0.042 (2) | 0.0219 (19) | −0.0080 (18) | −0.0055 (15) | 0.0113 (18) |
C25 | 0.031 (2) | 0.034 (2) | 0.0212 (18) | −0.0110 (17) | 0.0038 (15) | −0.0035 (16) |
C26 | 0.0209 (17) | 0.0206 (18) | 0.0252 (18) | −0.0030 (14) | 0.0051 (14) | −0.0007 (14) |
C27 | 0.0213 (17) | 0.0238 (18) | 0.0263 (19) | 0.0030 (14) | 0.0099 (15) | −0.0041 (15) |
C28 | 0.0193 (18) | 0.043 (2) | 0.032 (2) | −0.0063 (17) | 0.0092 (16) | −0.0061 (18) |
Pt1—P1 | 2.2633 (9) | C13—H13A | 0.99 |
Pt1—P2 | 2.2517 (9) | C13—H13B | 0.99 |
Pt1—Cl1 | 2.3458 (9) | C14—H14A | 0.98 |
Pt1—Cl2 | 2.3618 (9) | C14—H14B | 0.98 |
P1—C1 | 1.824 (3) | C14—H14C | 0.98 |
P1—C13 | 1.830 (4) | C15—C16 | 1.391 (5) |
P1—C7 | 1.832 (4) | C15—C20 | 1.397 (5) |
P2—C21 | 1.816 (4) | C16—C17 | 1.394 (5) |
P2—C15 | 1.820 (4) | C16—H16 | 0.95 |
P2—C27 | 1.835 (4) | C17—C18 | 1.391 (6) |
C1—C6 | 1.391 (5) | C17—H17 | 0.95 |
C1—C2 | 1.398 (5) | C18—C19 | 1.376 (6) |
C2—C3 | 1.387 (5) | C18—H18 | 0.95 |
C2—H2 | 0.95 | C19—C20 | 1.390 (5) |
C3—C4 | 1.386 (6) | C19—H19 | 0.95 |
C3—H3 | 0.95 | C20—H20 | 0.95 |
C4—C5 | 1.385 (6) | C21—C26 | 1.396 (5) |
C4—H4 | 0.95 | C21—C22 | 1.403 (5) |
C5—C6 | 1.394 (5) | C22—C23 | 1.388 (6) |
C5—H5 | 0.95 | C22—H22 | 0.95 |
C6—H6 | 0.95 | C23—C24 | 1.379 (7) |
C7—C12 | 1.395 (5) | C23—H23 | 0.95 |
C7—C8 | 1.400 (5) | C24—C25 | 1.390 (6) |
C8—C9 | 1.388 (6) | C24—H24 | 0.95 |
C8—H8 | 0.95 | C25—C26 | 1.395 (5) |
C9—C10 | 1.385 (7) | C25—H25 | 0.95 |
C9—H9 | 0.95 | C26—H26 | 0.95 |
C10—C11 | 1.386 (7) | C27—C28 | 1.537 (5) |
C10—H10 | 0.95 | C27—H27A | 0.99 |
C11—C12 | 1.397 (5) | C27—H27B | 0.99 |
C11—H11 | 0.95 | C28—H28A | 0.98 |
C12—H12 | 0.95 | C28—H28B | 0.98 |
C13—C14 | 1.529 (5) | C28—H28C | 0.98 |
P2—Pt1—P1 | 100.23 (3) | C14—C13—H13B | 108.9 |
P2—Pt1—Cl1 | 91.45 (3) | P1—C13—H13B | 108.9 |
P1—Pt1—Cl1 | 167.54 (3) | H13A—C13—H13B | 107.7 |
P2—Pt1—Cl2 | 175.70 (3) | C13—C14—H14A | 109.5 |
P1—Pt1—Cl2 | 82.81 (3) | C13—C14—H14B | 109.5 |
Cl1—Pt1—Cl2 | 85.30 (3) | H14A—C14—H14B | 109.5 |
C1—P1—C13 | 105.86 (17) | C13—C14—H14C | 109.5 |
C1—P1—C7 | 103.62 (15) | H14A—C14—H14C | 109.5 |
C13—P1—C7 | 102.95 (17) | H14B—C14—H14C | 109.5 |
C1—P1—Pt1 | 110.29 (12) | C16—C15—C20 | 118.7 (3) |
C13—P1—Pt1 | 108.86 (13) | C16—C15—P2 | 124.8 (3) |
C7—P1—Pt1 | 123.80 (11) | C20—C15—P2 | 116.6 (3) |
C21—P2—C15 | 106.63 (16) | C15—C16—C17 | 120.4 (3) |
C21—P2—C27 | 100.27 (17) | C15—C16—H16 | 119.8 |
C15—P2—C27 | 100.92 (17) | C17—C16—H16 | 119.8 |
C21—P2—Pt1 | 119.05 (12) | C18—C17—C16 | 120.0 (4) |
C15—P2—Pt1 | 112.12 (11) | C18—C17—H17 | 120 |
C27—P2—Pt1 | 115.72 (13) | C16—C17—H17 | 120 |
C6—C1—C2 | 118.8 (3) | C19—C18—C17 | 120.1 (4) |
C6—C1—P1 | 120.9 (3) | C19—C18—H18 | 120 |
C2—C1—P1 | 120.3 (3) | C17—C18—H18 | 120 |
C3—C2—C1 | 120.6 (4) | C18—C19—C20 | 119.9 (4) |
C3—C2—H2 | 119.7 | C18—C19—H19 | 120 |
C1—C2—H2 | 119.7 | C20—C19—H19 | 120 |
C4—C3—C2 | 120.2 (4) | C19—C20—C15 | 120.9 (4) |
C4—C3—H3 | 119.9 | C19—C20—H20 | 119.6 |
C2—C3—H3 | 119.9 | C15—C20—H20 | 119.6 |
C5—C4—C3 | 119.7 (4) | C26—C21—C22 | 119.2 (3) |
C5—C4—H4 | 120.1 | C26—C21—P2 | 120.9 (3) |
C3—C4—H4 | 120.1 | C22—C21—P2 | 119.5 (3) |
C4—C5—C6 | 120.2 (4) | C23—C22—C21 | 119.7 (4) |
C4—C5—H5 | 119.9 | C23—C22—H22 | 120.2 |
C6—C5—H5 | 119.9 | C21—C22—H22 | 120.2 |
C1—C6—C5 | 120.5 (4) | C24—C23—C22 | 121.1 (4) |
C1—C6—H6 | 119.8 | C24—C23—H23 | 119.4 |
C5—C6—H6 | 119.8 | C22—C23—H23 | 119.4 |
C12—C7—C8 | 118.4 (3) | C23—C24—C25 | 119.7 (4) |
C12—C7—P1 | 119.4 (3) | C23—C24—H24 | 120.2 |
C8—C7—P1 | 122.2 (3) | C25—C24—H24 | 120.2 |
C9—C8—C7 | 120.6 (4) | C24—C25—C26 | 119.9 (4) |
C9—C8—H8 | 119.7 | C24—C25—H25 | 120 |
C7—C8—H8 | 119.7 | C26—C25—H25 | 120 |
C10—C9—C8 | 120.5 (4) | C25—C26—C21 | 120.4 (4) |
C10—C9—H9 | 119.8 | C25—C26—H26 | 119.8 |
C8—C9—H9 | 119.8 | C21—C26—H26 | 119.8 |
C9—C10—C11 | 119.8 (4) | C28—C27—P2 | 115.4 (3) |
C9—C10—H10 | 120.1 | C28—C27—H27A | 108.4 |
C11—C10—H10 | 120.1 | P2—C27—H27A | 108.4 |
C10—C11—C12 | 120.0 (4) | C28—C27—H27B | 108.4 |
C10—C11—H11 | 120 | P2—C27—H27B | 108.4 |
C12—C11—H11 | 120 | H27A—C27—H27B | 107.5 |
C7—C12—C11 | 120.7 (4) | C27—C28—H28A | 109.5 |
C7—C12—H12 | 119.7 | C27—C28—H28B | 109.5 |
C11—C12—H12 | 119.7 | H28A—C28—H28B | 109.5 |
C14—C13—P1 | 113.4 (3) | C27—C28—H28C | 109.5 |
C14—C13—H13A | 108.9 | H28A—C28—H28C | 109.5 |
P1—C13—H13A | 108.9 | H28B—C28—H28C | 109.5 |
P2—Pt1—P1—C1 | 125.44 (12) | C7—C8—C9—C10 | −2.3 (6) |
Cl1—Pt1—P1—C1 | −75.1 (2) | C8—C9—C10—C11 | 2.2 (7) |
Cl2—Pt1—P1—C1 | −57.64 (13) | C9—C10—C11—C12 | 0.9 (7) |
P2—Pt1—P1—C13 | −118.82 (13) | C8—C7—C12—C11 | 3.9 (5) |
Cl1—Pt1—P1—C13 | 40.6 (2) | P1—C7—C12—C11 | −177.6 (3) |
Cl2—Pt1—P1—C13 | 58.09 (14) | C10—C11—C12—C7 | −4.0 (6) |
P2—Pt1—P1—C7 | 2.09 (14) | C1—P1—C13—C14 | 167.9 (3) |
Cl1—Pt1—P1—C7 | 161.55 (18) | C7—P1—C13—C14 | −83.7 (3) |
Cl2—Pt1—P1—C7 | 179.01 (14) | Pt1—P1—C13—C14 | 49.3 (3) |
P1—Pt1—P2—C21 | −67.66 (14) | C21—P2—C15—C16 | 19.0 (4) |
Cl1—Pt1—P2—C21 | 116.69 (14) | C27—P2—C15—C16 | 123.3 (3) |
Cl2—Pt1—P2—C21 | 157.7 (4) | Pt1—P2—C15—C16 | −112.9 (3) |
P1—Pt1—P2—C15 | 57.73 (13) | C21—P2—C15—C20 | −159.4 (3) |
Cl1—Pt1—P2—C15 | −117.92 (13) | C27—P2—C15—C20 | −55.1 (3) |
Cl2—Pt1—P2—C15 | −76.9 (5) | Pt1—P2—C15—C20 | 68.7 (3) |
P1—Pt1—P2—C27 | 172.74 (14) | C20—C15—C16—C17 | 2.6 (5) |
Cl1—Pt1—P2—C27 | −2.92 (14) | P2—C15—C16—C17 | −175.7 (3) |
Cl2—Pt1—P2—C27 | 38.1 (5) | C15—C16—C17—C18 | −0.2 (6) |
C13—P1—C1—C6 | −146.9 (3) | C16—C17—C18—C19 | −2.5 (6) |
C7—P1—C1—C6 | 105.2 (3) | C17—C18—C19—C20 | 2.8 (6) |
Pt1—P1—C1—C6 | −29.3 (3) | C18—C19—C20—C15 | −0.3 (7) |
C13—P1—C1—C2 | 32.5 (3) | C16—C15—C20—C19 | −2.3 (6) |
C7—P1—C1—C2 | −75.5 (3) | P2—C15—C20—C19 | 176.1 (3) |
Pt1—P1—C1—C2 | 150.1 (3) | C15—P2—C21—C26 | −138.3 (3) |
C6—C1—C2—C3 | −0.2 (5) | C27—P2—C21—C26 | 117.0 (3) |
P1—C1—C2—C3 | −179.6 (3) | Pt1—P2—C21—C26 | −10.3 (3) |
C1—C2—C3—C4 | −1.1 (6) | C15—P2—C21—C22 | 49.4 (3) |
C2—C3—C4—C5 | 1.4 (6) | C27—P2—C21—C22 | −55.4 (3) |
C3—C4—C5—C6 | −0.5 (6) | Pt1—P2—C21—C22 | 177.3 (3) |
C2—C1—C6—C5 | 1.1 (6) | C26—C21—C22—C23 | 1.3 (6) |
P1—C1—C6—C5 | −179.5 (3) | P2—C21—C22—C23 | 173.9 (3) |
C4—C5—C6—C1 | −0.8 (6) | C21—C22—C23—C24 | 0.2 (6) |
C1—P1—C7—C12 | −58.4 (3) | C22—C23—C24—C25 | −0.6 (7) |
C13—P1—C7—C12 | −168.6 (3) | C23—C24—C25—C26 | −0.7 (6) |
Pt1—P1—C7—C12 | 67.8 (3) | C24—C25—C26—C21 | 2.3 (6) |
C1—P1—C7—C8 | 120.0 (3) | C22—C21—C26—C25 | −2.6 (6) |
C13—P1—C7—C8 | 9.8 (3) | P2—C21—C26—C25 | −175.0 (3) |
Pt1—P1—C7—C8 | −113.8 (3) | C21—P2—C27—C28 | −51.3 (3) |
C12—C7—C8—C9 | −0.8 (6) | C15—P2—C27—C28 | −160.6 (3) |
P1—C7—C8—C9 | −179.2 (3) | Pt1—P2—C27—C28 | 78.1 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
C13—H13B···Cl2 | 0.99 | 2.78 | 3.278 (4) | 112 |
C18—H18···Cl2i | 0.95 | 2.75 | 3.539 (4) | 141 |
C27—H27A···Cl1ii | 0.99 | 2.74 | 3.622 (4) | 149 |
C27—H27B···Cl1 | 0.99 | 2.74 | 3.185 (4) | 108 |
C28—H28A···Cl1 | 0.98 | 2.70 | 3.373 (5) | 126 |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [PtCl2(C14H15P)2] |
Mr | 694.45 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 120 |
a, b, c (Å) | 14.2831 (6), 11.1025 (5), 16.9556 (7) |
β (°) | 106.677 (4) |
V (Å3) | 2575.69 (19) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.80 |
Crystal size (mm) | 0.26 × 0.14 × 0.07 |
Data collection | |
Diffractometer | Oxford Diffraction KM-4-CCD |
Absorption correction | Analytical CrysAlis RED (Oxford Diffraction, 2006; Clark & Reid, 1995). |
Tmin, Tmax | 0.232, 0.501 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 19512, 5614, 5413 |
Rint | 0.032 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.072, 1.10 |
No. of reflections | 5614 |
No. of parameters | 300 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.88, −1.23 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), CrysAlis RED, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999) and PLATON (Spek, 2003).
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In the course of our studies upon the reactivity of [(R3P)2MCl2] towards R'2P–P(SiMe3)2 (Domańska-Babul et al., 2007) we have studied the reaction of (iPr2N)2P–P(SiMe3)2 with [(EtPh2P)2PtCl2]. The title compound was obtained unchanged in the synthesis.
The complex exhibits square-planar coordination that is typical for platinum(II) compounds. The platinum atom is 0.0556 (4) Å above the square plane. The structure is similar to that of [(MePh2P)2PtCl2] (Ho et al., 1982). The square planar geometry is characteristic of complexes having less bulky tertiary phosphines. Significant deviation from planarity is observed with sterically bulky phosphines ligands, as noted in cis-dichlorobis(di-t-butylphenylphosphine)platinum(II) (Krautscheid et al., 1997; Porzio et al., 1980). The bond dimensions involving the platinum atom are typical of [cis-(R3P)2PtCl2] compounds such as for [(MePh2P)2PtCl2]. Weak intermolecular C—H···Cl interactions are also present.