Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807030966/gg2016sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807030966/gg2016Isup2.hkl |
CCDC reference: 654838
Key indicators
- Single-crystal X-ray study
- T = 125 K
- Mean (C-C) = 0.005 Å
- R factor = 0.021
- wR factor = 0.043
- Data-to-parameter ratio = 16.0
checkCIF/PLATON results
No syntax errors found
Alert level A DIFF019_ALERT_1_A _diffrn_standards_number is missing Number of standards used in measurement. DIFF020_ALERT_1_A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards. DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing Percentage decrease in standards intensity.
3 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related literature on PtCl2L2 complexes, see: Bao et al. (1987); Fun et al. (2006); Slawin et al. (2007).
1 g (2.67 mmol) of PtCl2(COD) was dissolved in the minimum volume of dichloromethane in a round-bottomed flask. To this, 0.840 ml (5.34 mmol) of dimethylphenylphosphonite was added. The solution was then stirred for 0.5 h at room temperature. The product was precipitated via slow diffusion of hexane and was then filtered off and dried under vacuum, [PtCl2(P(OMe)2Ph)2] (1.86 mmol,ca 69%). 31P-{1H} NMR: δ 91.2 p.p.m. J{Pt—P} 4819 Hz.
All H atoms were included in calculated positions (C—H distances are 0.96 Å for methyl H atoms, 0.97 Å for methylene H atoms and 0.98 Å for methine H atoms) and were refined as riding atoms with Uiso(H) = 1.2 Ueq(parent atom, methylene and methine H atoms) or Uiso(H) = 1.5 Ueq(parent atom, methyl H atoms).
The title complex (I) is comparable to similar platinum dichloride complexes containing trimethoxy phosphite; [PtCl2(P(OMe)3)2] (Bao et al., 1987) and triphenyl phosphine [PtCl2(PPh3)2] (Fun et al., 2006). The central platinum atom in (I) can be seen to bear a closer resemblance to the triphenyl phosphine complex. These measurement are also similar when compared to the structure of the complex [PtCl2(P(OMe)Ph2)2] (Slawin et al., 2007) with the exception of the P—Pt—P bond angle which is unusually large.
For related literature on PtCl2L2 complexes, see: Bao et al. (1987); Fun et al. (2006); Slawin et al. (2007).
Data collection: SCXmini (Rigaku/MSC, 2006); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalStructure (Rigaku/MSC, 2006); software used to prepare material for publication: CrystalStructure.
Fig. 1. The structure of (1) with displacement ellipsoids drawn at the 50% probability level, H atoms omitted for clarity. |
[PtCl2(C8H11O2P)2] | F(000) = 1168 |
Mr = 606.27 | Dx = 1.967 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 6759 reflections |
a = 10.9734 (7) Å | θ = 3.0–27.5° |
b = 9.2290 (6) Å | µ = 7.29 mm−1 |
c = 20.7002 (14) Å | T = 125 K |
β = 102.398 (2)° | Prism, colourless |
V = 2047.5 (2) Å3 | 0.20 × 0.16 × 0.07 mm |
Z = 4 |
Rigaku SCXmini diffractometer | 1869 independent reflections |
Radiation source: fine-focus sealed tube | 1772 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ω scans | θmax = 25.3°, θmin = 3.2° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −13→13 |
Tmin = 0.261, Tmax = 0.602 | k = −11→10 |
5869 measured reflections | l = −24→24 |
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)] = 0.021 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.043 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0167P)2 + 0.5089P] where P = (Fo2 + 2Fc2)/3 |
1869 reflections | (Δ/σ)max = 0.007 |
117 parameters | Δρmax = 0.62 e Å−3 |
0 restraints | Δρmin = −0.69 e Å−3 |
[PtCl2(C8H11O2P)2] | V = 2047.5 (2) Å3 |
Mr = 606.27 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.9734 (7) Å | µ = 7.29 mm−1 |
b = 9.2290 (6) Å | T = 125 K |
c = 20.7002 (14) Å | 0.20 × 0.16 × 0.07 mm |
β = 102.398 (2)° |
Rigaku SCXmini diffractometer | 1869 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 1772 reflections with I > 2σ(I) |
Tmin = 0.261, Tmax = 0.602 | Rint = 0.035 |
5869 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 0 restraints |
wR(F2) = 0.043 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.62 e Å−3 |
1869 reflections | Δρmin = −0.69 e Å−3 |
117 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 | 0.5000 | 0.40682 (2) | 0.2500 | 0.01234 (7) | |
Cl1 | 0.59209 (8) | 0.58930 (10) | 0.32480 (4) | 0.0204 (2) | |
P1 | 0.40029 (8) | 0.25413 (10) | 0.17390 (4) | 0.0141 (2) | |
C1 | 0.4614 (3) | 0.2496 (4) | 0.09966 (17) | 0.0156 (8) | |
C2 | 0.4028 (3) | 0.3176 (4) | 0.04180 (18) | 0.0217 (9) | |
H2A | 0.3264 | 0.3677 | 0.0397 | 0.026* | |
C3 | 0.4560 (3) | 0.3125 (5) | −0.01343 (19) | 0.0270 (10) | |
H3A | 0.4166 | 0.3598 | −0.0532 | 0.032* | |
C4 | 0.5671 (4) | 0.2379 (4) | −0.01014 (19) | 0.0300 (10) | |
H4A | 0.6027 | 0.2337 | −0.0481 | 0.036* | |
C5 | 0.6258 (4) | 0.1707 (5) | 0.0466 (2) | 0.0314 (10) | |
H5A | 0.7017 | 0.1200 | 0.0480 | 0.038* | |
C6 | 0.5744 (3) | 0.1764 (4) | 0.10287 (19) | 0.0244 (9) | |
H6A | 0.6158 | 0.1312 | 0.1428 | 0.029* | |
O1 | 0.3959 (2) | 0.0909 (2) | 0.19814 (12) | 0.0195 (6) | |
C7 | 0.3218 (4) | −0.0145 (4) | 0.15439 (19) | 0.0261 (9) | |
H7A | 0.2341 | −0.0059 | 0.1573 | 0.039* | |
H7B | 0.3518 | −0.1124 | 0.1676 | 0.039* | |
H7C | 0.3294 | 0.0037 | 0.1088 | 0.039* | |
O2 | 0.2590 (2) | 0.2966 (3) | 0.14365 (11) | 0.0170 (5) | |
C8 | 0.1756 (3) | 0.3272 (5) | 0.18759 (19) | 0.0266 (10) | |
H8A | 0.1804 | 0.2485 | 0.2198 | 0.040* | |
H8B | 0.0899 | 0.3353 | 0.1617 | 0.040* | |
H8C | 0.2001 | 0.4185 | 0.2109 | 0.040* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.01451 (11) | 0.01079 (12) | 0.01187 (12) | 0.000 | 0.00317 (8) | 0.000 |
Cl1 | 0.0245 (5) | 0.0150 (5) | 0.0195 (5) | −0.0003 (4) | −0.0004 (4) | −0.0036 (4) |
P1 | 0.0172 (5) | 0.0127 (5) | 0.0125 (5) | −0.0014 (4) | 0.0033 (4) | 0.0006 (4) |
C1 | 0.0178 (17) | 0.012 (2) | 0.017 (2) | −0.0047 (14) | 0.0040 (16) | −0.0026 (15) |
C2 | 0.022 (2) | 0.023 (2) | 0.019 (2) | 0.0008 (16) | 0.0039 (18) | −0.0017 (17) |
C3 | 0.031 (2) | 0.035 (3) | 0.012 (2) | −0.0028 (19) | −0.0005 (18) | 0.0011 (18) |
C4 | 0.037 (2) | 0.036 (3) | 0.020 (2) | −0.003 (2) | 0.012 (2) | −0.0060 (19) |
C5 | 0.023 (2) | 0.040 (3) | 0.034 (3) | 0.0069 (19) | 0.013 (2) | 0.001 (2) |
C6 | 0.024 (2) | 0.027 (2) | 0.022 (2) | 0.0081 (17) | 0.0031 (18) | 0.0058 (18) |
O1 | 0.0272 (13) | 0.0134 (14) | 0.0167 (14) | −0.0058 (11) | 0.0021 (11) | −0.0003 (11) |
C7 | 0.040 (2) | 0.015 (2) | 0.022 (2) | −0.0068 (18) | 0.004 (2) | −0.0039 (17) |
O2 | 0.0157 (12) | 0.0190 (15) | 0.0167 (14) | −0.0006 (10) | 0.0048 (11) | −0.0002 (11) |
C8 | 0.022 (2) | 0.031 (3) | 0.030 (2) | −0.0002 (17) | 0.0135 (19) | 0.0001 (19) |
Pt1—P1 | 2.2190 (9) | C4—C5 | 1.362 (5) |
Pt1—P1i | 2.2190 (9) | C4—H4A | 0.9500 |
Pt1—Cl1 | 2.3629 (9) | C5—C6 | 1.400 (5) |
Pt1—Cl1i | 2.3629 (9) | C5—H5A | 0.9500 |
P1—O1 | 1.592 (2) | C6—H6A | 0.9500 |
P1—O2 | 1.591 (2) | O1—C7 | 1.453 (4) |
P1—C1 | 1.804 (3) | C7—H7A | 0.9800 |
C1—C2 | 1.382 (5) | C7—H7B | 0.9800 |
C1—C6 | 1.402 (5) | C7—H7C | 0.9800 |
C2—C3 | 1.392 (5) | O2—C8 | 1.450 (4) |
C2—H2A | 0.9500 | C8—H8A | 0.9800 |
C3—C4 | 1.388 (5) | C8—H8B | 0.9800 |
C3—H3A | 0.9500 | C8—H8C | 0.9800 |
P1—Pt1—P1i | 101.16 (5) | C5—C4—H4A | 119.5 |
P1—Pt1—Cl1 | 173.78 (3) | C3—C4—H4A | 119.5 |
P1i—Pt1—Cl1 | 84.90 (3) | C4—C5—C6 | 120.0 (4) |
P1—Pt1—Cl1i | 84.90 (3) | C4—C5—H5A | 120.0 |
P1i—Pt1—Cl1i | 173.78 (3) | C6—C5—H5A | 120.0 |
Cl1—Pt1—Cl1i | 89.08 (4) | C5—C6—C1 | 119.3 (4) |
O1—P1—O2 | 105.34 (13) | C5—C6—H6A | 120.3 |
O1—P1—C1 | 106.75 (15) | C1—C6—H6A | 120.3 |
O2—P1—C1 | 100.32 (14) | C7—O1—P1 | 119.2 (2) |
O1—P1—Pt1 | 114.89 (10) | O1—C7—H7A | 109.5 |
O2—P1—Pt1 | 114.40 (10) | O1—C7—H7B | 109.5 |
C1—P1—Pt1 | 113.76 (11) | H7A—C7—H7B | 109.5 |
C2—C1—C6 | 120.1 (3) | O1—C7—H7C | 109.5 |
C2—C1—P1 | 122.6 (3) | H7A—C7—H7C | 109.5 |
C6—C1—P1 | 117.3 (3) | H7B—C7—H7C | 109.5 |
C1—C2—C3 | 119.8 (3) | C8—O2—P1 | 119.6 (2) |
C1—C2—H2A | 120.1 | O2—C8—H8A | 109.5 |
C3—C2—H2A | 120.1 | O2—C8—H8B | 109.5 |
C4—C3—C2 | 119.7 (4) | H8A—C8—H8B | 109.5 |
C4—C3—H3A | 120.2 | O2—C8—H8C | 109.5 |
C2—C3—H3A | 120.2 | H8A—C8—H8C | 109.5 |
C5—C4—C3 | 121.1 (4) | H8B—C8—H8C | 109.5 |
P1i—Pt1—P1—O1 | 14.27 (10) | P1—C1—C2—C3 | 178.7 (3) |
Cl1i—Pt1—P1—O1 | −167.15 (11) | C1—C2—C3—C4 | 0.6 (6) |
P1i—Pt1—P1—O2 | 136.32 (11) | C2—C3—C4—C5 | −0.7 (6) |
Cl1i—Pt1—P1—O2 | −45.10 (10) | C3—C4—C5—C6 | −0.1 (7) |
P1i—Pt1—P1—C1 | −109.19 (13) | C4—C5—C6—C1 | 1.1 (6) |
Cl1i—Pt1—P1—C1 | 69.39 (13) | C2—C1—C6—C5 | −1.3 (6) |
O1—P1—C1—C2 | 129.0 (3) | P1—C1—C6—C5 | −179.6 (3) |
O2—P1—C1—C2 | 19.4 (3) | O2—P1—O1—C7 | 46.7 (3) |
Pt1—P1—C1—C2 | −103.2 (3) | C1—P1—O1—C7 | −59.3 (3) |
O1—P1—C1—C6 | −52.7 (3) | Pt1—P1—O1—C7 | 173.6 (2) |
O2—P1—C1—C6 | −162.3 (3) | O1—P1—O2—C8 | 75.5 (3) |
Pt1—P1—C1—C6 | 75.1 (3) | C1—P1—O2—C8 | −173.8 (3) |
C6—C1—C2—C3 | 0.4 (5) | Pt1—P1—O2—C8 | −51.6 (3) |
Symmetry code: (i) −x+1, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C7—H7B···Cl1ii | 0.98 | 2.82 | 3.778 (4) | 166 |
Symmetry code: (ii) −x+1, y−1, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [PtCl2(C8H11O2P)2] |
Mr | 606.27 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 125 |
a, b, c (Å) | 10.9734 (7), 9.2290 (6), 20.7002 (14) |
β (°) | 102.398 (2) |
V (Å3) | 2047.5 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 7.29 |
Crystal size (mm) | 0.20 × 0.16 × 0.07 |
Data collection | |
Diffractometer | Rigaku SCXmini |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.261, 0.602 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5869, 1869, 1772 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.602 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.043, 1.07 |
No. of reflections | 1869 |
No. of parameters | 117 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.62, −0.69 |
Computer programs: SCXmini (Rigaku/MSC, 2006), PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), CrystalStructure (Rigaku/MSC, 2006), CrystalStructure.
Pt1—P1 | 2.2190 (9) | Pt1—Cl1 | 2.3629 (9) |
P1—Pt1—P1i | 101.16 (5) | P1i—Pt1—Cl1 | 84.90 (3) |
P1—Pt1—Cl1 | 173.78 (3) | Cl1—Pt1—Cl1i | 89.08 (4) |
Symmetry code: (i) −x+1, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C7—H7B···Cl1ii | 0.98 | 2.82 | 3.778 (4) | 166 |
Symmetry code: (ii) −x+1, y−1, −z+1/2. |
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The title complex (I) is comparable to similar platinum dichloride complexes containing trimethoxy phosphite; [PtCl2(P(OMe)3)2] (Bao et al., 1987) and triphenyl phosphine [PtCl2(PPh3)2] (Fun et al., 2006). The central platinum atom in (I) can be seen to bear a closer resemblance to the triphenyl phosphine complex. These measurement are also similar when compared to the structure of the complex [PtCl2(P(OMe)Ph2)2] (Slawin et al., 2007) with the exception of the P—Pt—P bond angle which is unusually large.