supplementary materials
Dichloridobis(2-methoxydibenzo[c,e][1,2]oxaphosphorine-
P)platinum(II) trichloromethane solvate
Synthesis of the parent compound and related ones is reported by Keglevich
et al. (2008). Recrystallization of the title
dibenzo-oxaphosphorine
complex from chloroform yielded X-ray quality crystals, solvent content of
which became apparent only after the X-ray study.
H atoms were placed in idealized positions (C-H = 0.95-0.98 Å) and refined
using a riding model with Uiso(H) = 1.2-1.5Ueq(C). The Cl atoms of the
trichloromethane solvent molecule were disordered over two sites.
The site occupancies and displacement parameters of the disordered atoms were
alternately refined and during the final cycles of refinement the occupancies
were fixed at 0.75 and 0.25. The C—Cl and Cl···Cl distances involving the
disordered atoms were restrained to be equal, and also their Uij parameters
were restrained to an approximate isotropic behaviour. The free and restrained
refinement models for the solvent resulted in small differences in occupancies
of chlorine sites. The restraints virtually improved C—Cl and C···C distances
but the maximum positive residual peak appeared close to a minor occupancy Cl
site in contrast to the free disorder model, where both maximum and minimum
residual densities appeared close to the metal atom.
Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009).
Dichloridobis(2-methoxydibenzo[c,e][1,2]oxaphosphorine-
κP)platinum(II)
trichloromethane solvate
top
Crystal data top
| [PtCl2(C13H11O2P)2]·CHCl3 | Z = 2 |
| Mr = 845.73 | F(000) = 820 |
| Triclinic, P1 | Dx = 1.920 Mg m−3 |
| Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71070 Å |
| a = 10.186 (3) Å | Cell parameters from 40740 reflections |
| b = 13.020 (5) Å | θ = 3.1–28.7° |
| c = 13.510 (5) Å | µ = 5.40 mm−1 |
| α = 62.402 (11)° | T = 93 K |
| β = 83.128 (12)° | Prism, colourless |
| γ = 67.456 (11)° | 0.40 × 0.30 × 0.15 mm |
| V = 1462.8 (9) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 5339 independent reflections |
| Radiation source: fine-focus sealed tube | 4822 reflections with I > 2σ(I) |
| graphite | Rint = 0.114 |
| Detector resolution: 10 pixels mm-1 | θmax = 25.4°, θmin = 3.1° |
| ω scans | h = −12→12 |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008) | k = −15→15 |
| Tmin = 0.222, Tmax = 0.498 | l = −16→16 |
| 36911 measured reflections | |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.151 | H-atom parameters constrained |
| S = 1.06 | w = 1/[σ2(Fo2) + (0.0609P)2 + 24.9249P] where P = (Fo2 + 2Fc2)/3 |
| 5339 reflections | (Δ/σ)max = 0.001 |
| 381 parameters | Δρmax = 3.66 e Å−3 |
| 66 restraints | Δρmin = −2.69 e Å−3 |
Crystal data top
| [PtCl2(C13H11O2P)2]·CHCl3 | γ = 67.456 (11)° |
| Mr = 845.73 | V = 1462.8 (9) Å3 |
| Triclinic, P1 | Z = 2 |
| a = 10.186 (3) Å | Mo Kα radiation |
| b = 13.020 (5) Å | µ = 5.40 mm−1 |
| c = 13.510 (5) Å | T = 93 K |
| α = 62.402 (11)° | 0.40 × 0.30 × 0.15 mm |
| β = 83.128 (12)° | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 5339 independent reflections |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008) | 4822 reflections with I > 2σ(I) |
| Tmin = 0.222, Tmax = 0.498 | Rint = 0.114 |
| 36911 measured reflections | θmax = 25.4° |
Refinement top
| R[F2 > 2σ(F2)] = 0.059 | w = 1/[σ2(Fo2) + (0.0609P)2 + 24.9249P] where P = (Fo2 + 2Fc2)/3 |
| wR(F2) = 0.151 | Δρmax = 3.66 e Å−3 |
| S = 1.06 | Δρmin = −2.69 e Å−3 |
| 5339 reflections | Absolute structure: ? |
| 381 parameters | Flack parameter: ? |
| 66 restraints | Rogers parameter: ? |
| H-atom parameters constrained | |
Special details top
Experimental. Multi-scan empirical absorption correction by T. Higashi in FS-Process |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top| | x | y | z | Uiso*/Ueq | Occ. (<1) |
| Pt1 | −0.03953 (4) | 0.00011 (3) | 0.72977 (3) | 0.02055 (16) | |
| Cl1 | −0.0887 (3) | −0.1812 (2) | 0.8105 (2) | 0.0269 (5) | |
| Cl2 | −0.2425 (3) | 0.0975 (3) | 0.6061 (2) | 0.0301 (6) | |
| P1 | −0.0015 (3) | 0.1747 (2) | 0.6439 (2) | 0.0217 (5) | |
| P2 | 0.1547 (3) | −0.0974 (2) | 0.8424 (2) | 0.0206 (5) | |
| O2 | −0.0202 (9) | 0.2390 (7) | 0.5122 (6) | 0.0282 (17) | |
| O1 | 0.1586 (8) | 0.1516 (6) | 0.6736 (6) | 0.0244 (15) | |
| O4 | 0.1766 (8) | −0.2306 (6) | 0.9426 (6) | 0.0244 (15) | |
| O3 | 0.1682 (7) | −0.0208 (6) | 0.9011 (6) | 0.0205 (14) | |
| C8 | −0.1302 (14) | 0.4864 (11) | 0.6809 (10) | 0.036 (3) | |
| H8 | −0.0918 | 0.5447 | 0.6755 | 0.043* | |
| C20 | 0.4336 (11) | −0.1284 (10) | 0.8228 (9) | 0.025 (2) | |
| C5 | 0.1658 (13) | 0.4537 (10) | 0.6086 (10) | 0.031 (2) | |
| H5 | 0.1062 | 0.5328 | 0.6039 | 0.037* | |
| C6 | 0.1065 (12) | 0.3635 (10) | 0.6376 (9) | 0.026 (2) | |
| C4 | 0.3042 (13) | 0.4330 (10) | 0.5870 (9) | 0.031 (3) | |
| H4 | 0.3392 | 0.4973 | 0.5683 | 0.038* | |
| C3 | 0.3947 (13) | 0.3213 (11) | 0.5916 (10) | 0.032 (3) | |
| H3 | 0.4913 | 0.3085 | 0.5751 | 0.039* | |
| C2 | 0.3439 (12) | 0.2267 (10) | 0.6208 (9) | 0.028 (2) | |
| H2 | 0.4050 | 0.1477 | 0.6261 | 0.034* | |
| C1 | 0.2005 (11) | 0.2512 (9) | 0.6421 (8) | 0.022 (2) | |
| C12 | −0.1048 (12) | 0.3029 (10) | 0.6709 (9) | 0.027 (2) | |
| C11 | −0.2464 (13) | 0.3206 (11) | 0.6967 (10) | 0.032 (3) | |
| H11 | −0.2855 | 0.2623 | 0.7034 | 0.039* | |
| C10 | −0.3290 (13) | 0.4235 (10) | 0.7126 (10) | 0.033 (3) | |
| H10 | −0.4261 | 0.4379 | 0.7282 | 0.040* | |
| C9 | −0.2690 (14) | 0.5046 (12) | 0.7054 (11) | 0.038 (3) | |
| H9 | −0.3249 | 0.5747 | 0.7176 | 0.045* | |
| C18 | 0.5477 (11) | −0.1675 (10) | 0.9975 (9) | 0.027 (2) | |
| H18 | 0.6385 | −0.2056 | 0.9761 | 0.033* | |
| C19 | 0.4259 (11) | −0.1218 (10) | 0.9284 (9) | 0.024 (2) | |
| C17 | 0.5387 (13) | −0.1583 (11) | 1.0952 (10) | 0.031 (2) | |
| H17 | 0.6228 | −0.1905 | 1.1409 | 0.037* | |
| C16 | 0.4095 (13) | −0.1031 (11) | 1.1274 (10) | 0.031 (2) | |
| H16 | 0.4044 | −0.0966 | 1.1951 | 0.038* | |
| C15 | 0.2862 (12) | −0.0566 (10) | 1.0621 (9) | 0.027 (2) | |
| H15 | 0.1961 | −0.0169 | 1.0834 | 0.032* | |
| C14 | 0.2973 (11) | −0.0692 (9) | 0.9645 (9) | 0.023 (2) | |
| C25 | 0.3171 (10) | −0.1268 (10) | 0.7759 (9) | 0.023 (2) | |
| C24 | 0.3216 (11) | −0.1342 (10) | 0.6771 (9) | 0.027 (2) | |
| H24 | 0.2402 | −0.1315 | 0.6468 | 0.032* | |
| C23 | 0.4470 (13) | −0.1458 (12) | 0.6224 (10) | 0.036 (3) | |
| H23 | 0.4530 | −0.1535 | 0.5552 | 0.044* | |
| C22 | 0.5620 (12) | −0.1459 (12) | 0.6658 (10) | 0.035 (3) | |
| H22 | 0.6466 | −0.1514 | 0.6270 | 0.042* | |
| C7 | −0.0446 (12) | 0.3848 (10) | 0.6641 (9) | 0.027 (2) | |
| C13 | 0.0389 (14) | 0.1694 (12) | 0.4507 (11) | 0.037 (3) | |
| H13A | 0.1365 | 0.1117 | 0.4811 | 0.055* | |
| H13B | 0.0399 | 0.2267 | 0.3718 | 0.055* | |
| H13C | −0.0191 | 0.1218 | 0.4570 | 0.055* | |
| C21 | 0.5574 (12) | −0.1384 (11) | 0.7646 (10) | 0.032 (3) | |
| H21 | 0.6391 | −0.1399 | 0.7936 | 0.038* | |
| C26 | 0.0861 (14) | −0.2423 (11) | 1.0352 (10) | 0.035 (3) | |
| H26A | −0.0134 | −0.2095 | 1.0075 | 0.053* | |
| H26B | 0.0965 | −0.1949 | 1.0708 | 0.053* | |
| H26C | 0.1140 | −0.3305 | 1.0901 | 0.053* | |
| C27 | 0.7983 (12) | 0.4650 (12) | 0.0943 (6) | 0.063 (5) | |
| H27 | 0.8702 | 0.3883 | 0.0978 | 0.076* | |
| Cl3A | 0.8930 (6) | 0.5478 (5) | 0.1096 (5) | 0.0597 (13) | 0.75 |
| Cl4A | 0.7076 (9) | 0.5499 (5) | −0.0314 (5) | 0.096 (3) | 0.75 |
| Cl5A | 0.7023 (7) | 0.4234 (6) | 0.2081 (6) | 0.092 (2) | 0.75 |
| Cl3B | 0.6172 (15) | 0.478 (2) | 0.0820 (17) | 0.115 (8) | 0.25 |
| Cl4B | 0.801 (2) | 0.519 (2) | 0.1872 (13) | 0.101 (7) | 0.25 |
| Cl5B | 0.8268 (17) | 0.5635 (14) | −0.0399 (9) | 0.067 (4) | 0.25 |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| Pt1 | 0.0207 (2) | 0.0197 (2) | 0.0229 (2) | −0.01008 (17) | 0.00217 (16) | −0.00909 (18) |
| Cl1 | 0.0273 (13) | 0.0263 (13) | 0.0306 (13) | −0.0164 (11) | 0.0015 (11) | −0.0105 (11) |
| Cl2 | 0.0258 (13) | 0.0334 (14) | 0.0328 (14) | −0.0082 (11) | −0.0027 (11) | −0.0174 (12) |
| P1 | 0.0233 (13) | 0.0177 (12) | 0.0222 (13) | −0.0071 (10) | 0.0002 (10) | −0.0077 (11) |
| P2 | 0.0224 (13) | 0.0187 (13) | 0.0246 (13) | −0.0110 (10) | 0.0037 (10) | −0.0107 (11) |
| O2 | 0.040 (4) | 0.028 (4) | 0.022 (4) | −0.016 (3) | 0.005 (3) | −0.013 (3) |
| O1 | 0.024 (4) | 0.017 (3) | 0.027 (4) | −0.008 (3) | −0.002 (3) | −0.005 (3) |
| O4 | 0.029 (4) | 0.019 (4) | 0.022 (4) | −0.011 (3) | −0.002 (3) | −0.005 (3) |
| O3 | 0.020 (3) | 0.026 (4) | 0.022 (4) | −0.010 (3) | −0.003 (3) | −0.014 (3) |
| C8 | 0.055 (8) | 0.023 (6) | 0.025 (6) | −0.011 (5) | −0.003 (5) | −0.009 (5) |
| C20 | 0.026 (5) | 0.020 (5) | 0.025 (5) | −0.009 (4) | 0.002 (4) | −0.008 (4) |
| C5 | 0.041 (7) | 0.021 (5) | 0.030 (6) | −0.014 (5) | −0.002 (5) | −0.009 (5) |
| C6 | 0.032 (6) | 0.024 (5) | 0.023 (5) | −0.013 (5) | 0.002 (4) | −0.009 (4) |
| C4 | 0.049 (7) | 0.011 (5) | 0.027 (6) | −0.014 (5) | −0.001 (5) | 0.000 (4) |
| C3 | 0.029 (6) | 0.041 (7) | 0.031 (6) | −0.023 (5) | 0.003 (5) | −0.011 (5) |
| C2 | 0.028 (6) | 0.027 (6) | 0.031 (6) | −0.013 (5) | 0.006 (5) | −0.014 (5) |
| C1 | 0.032 (6) | 0.019 (5) | 0.014 (5) | −0.015 (4) | −0.003 (4) | 0.000 (4) |
| C12 | 0.027 (6) | 0.024 (5) | 0.026 (5) | −0.007 (4) | 0.000 (4) | −0.009 (5) |
| C11 | 0.033 (6) | 0.035 (6) | 0.035 (6) | −0.016 (5) | 0.005 (5) | −0.020 (5) |
| C10 | 0.030 (6) | 0.024 (6) | 0.032 (6) | 0.001 (5) | 0.005 (5) | −0.012 (5) |
| C9 | 0.039 (7) | 0.032 (6) | 0.038 (7) | −0.008 (5) | −0.006 (5) | −0.015 (6) |
| C18 | 0.021 (5) | 0.028 (6) | 0.031 (6) | −0.009 (4) | 0.002 (4) | −0.012 (5) |
| C19 | 0.029 (6) | 0.022 (5) | 0.023 (5) | −0.016 (4) | 0.001 (4) | −0.007 (4) |
| C17 | 0.034 (6) | 0.027 (6) | 0.032 (6) | −0.011 (5) | −0.006 (5) | −0.012 (5) |
| C16 | 0.040 (7) | 0.033 (6) | 0.027 (6) | −0.020 (5) | 0.002 (5) | −0.013 (5) |
| C15 | 0.037 (6) | 0.026 (5) | 0.026 (5) | −0.019 (5) | 0.002 (5) | −0.013 (5) |
| C14 | 0.026 (5) | 0.010 (4) | 0.023 (5) | −0.008 (4) | −0.002 (4) | 0.002 (4) |
| C25 | 0.013 (5) | 0.024 (5) | 0.036 (6) | −0.008 (4) | 0.003 (4) | −0.016 (5) |
| C24 | 0.020 (5) | 0.029 (6) | 0.033 (6) | −0.008 (4) | −0.003 (4) | −0.016 (5) |
| C23 | 0.029 (6) | 0.052 (8) | 0.031 (6) | −0.011 (6) | 0.007 (5) | −0.026 (6) |
| C22 | 0.024 (6) | 0.051 (8) | 0.034 (6) | −0.014 (5) | 0.011 (5) | −0.024 (6) |
| C7 | 0.032 (6) | 0.021 (5) | 0.019 (5) | −0.005 (4) | −0.009 (4) | −0.004 (4) |
| C13 | 0.049 (7) | 0.039 (7) | 0.039 (7) | −0.025 (6) | 0.017 (6) | −0.027 (6) |
| C21 | 0.023 (5) | 0.033 (6) | 0.030 (6) | −0.010 (5) | −0.002 (5) | −0.006 (5) |
| C26 | 0.052 (8) | 0.032 (6) | 0.027 (6) | −0.027 (6) | 0.006 (5) | −0.010 (5) |
| C27 | 0.080 (12) | 0.027 (7) | 0.061 (10) | −0.004 (7) | 0.005 (9) | −0.016 (7) |
| Cl3A | 0.065 (3) | 0.056 (3) | 0.068 (3) | −0.030 (2) | 0.006 (3) | −0.030 (3) |
| Cl4A | 0.136 (6) | 0.050 (3) | 0.089 (4) | 0.004 (3) | −0.058 (4) | −0.038 (3) |
| Cl5A | 0.092 (4) | 0.077 (4) | 0.126 (6) | −0.049 (4) | 0.060 (4) | −0.059 (4) |
| Cl3B | 0.137 (13) | 0.104 (11) | 0.122 (12) | −0.043 (9) | 0.029 (9) | −0.072 (9) |
| Cl4B | 0.106 (11) | 0.095 (10) | 0.080 (10) | −0.006 (8) | 0.001 (8) | −0.047 (8) |
| Cl5B | 0.061 (8) | 0.054 (7) | 0.068 (8) | −0.015 (6) | 0.015 (7) | −0.023 (6) |
Geometric parameters (Å, °) top
| Pt1—P1 | 2.188 (3) | C10—C9 | 1.374 (18) |
| Pt1—P2 | 2.201 (3) | C10—H10 | 0.95 |
| Pt1—Cl1 | 2.325 (3) | C9—H9 | 0.95 |
| Pt1—Cl2 | 2.351 (3) | C18—C17 | 1.369 (16) |
| P1—O2 | 1.575 (8) | C18—C19 | 1.401 (15) |
| P1—O1 | 1.607 (7) | C18—H18 | 0.95 |
| P1—C12 | 1.775 (11) | C19—C14 | 1.376 (15) |
| P2—O4 | 1.579 (7) | C17—C16 | 1.365 (17) |
| P2—O3 | 1.584 (7) | C17—H17 | 0.95 |
| P2—C25 | 1.780 (10) | C16—C15 | 1.382 (16) |
| O2—C13 | 1.426 (13) | C16—H16 | 0.95 |
| O1—C1 | 1.383 (12) | C15—C14 | 1.389 (15) |
| O4—C26 | 1.446 (14) | C15—H15 | 0.95 |
| O3—C14 | 1.411 (12) | C25—C24 | 1.376 (15) |
| C8—C9 | 1.366 (18) | C24—C23 | 1.390 (16) |
| C8—C7 | 1.382 (16) | C24—H24 | 0.95 |
| C8—H8 | 0.95 | C23—C22 | 1.370 (17) |
| C20—C21 | 1.398 (15) | C23—H23 | 0.95 |
| C20—C25 | 1.400 (15) | C22—C21 | 1.378 (17) |
| C20—C19 | 1.459 (15) | C22—H22 | 0.95 |
| C5—C4 | 1.352 (17) | C13—H13A | 0.98 |
| C5—C6 | 1.399 (15) | C13—H13B | 0.98 |
| C5—H5 | 0.95 | C13—H13C | 0.98 |
| C6—C1 | 1.385 (15) | C21—H21 | 0.95 |
| C6—C7 | 1.486 (16) | C26—H26A | 0.98 |
| C4—C3 | 1.368 (17) | C26—H26B | 0.98 |
| C4—H4 | 0.95 | C26—H26C | 0.98 |
| C3—C2 | 1.389 (16) | C27—Cl4A | 1.676 (8) |
| C3—H3 | 0.95 | C27—Cl5A | 1.700 (8) |
| C2—C1 | 1.394 (15) | C27—Cl4B | 1.705 (9) |
| C2—H2 | 0.95 | C27—Cl5B | 1.738 (9) |
| C12—C7 | 1.386 (16) | C27—Cl3A | 1.785 (8) |
| C12—C11 | 1.398 (16) | C27—Cl3B | 1.807 (10) |
| C11—C10 | 1.380 (16) | C27—H27 | 0.97 |
| C11—H11 | 0.95 | | |
| | | |
| P1—Pt1—P2 | 93.21 (10) | C17—C18—H18 | 119.3 |
| P1—Pt1—Cl1 | 176.23 (9) | C19—C18—H18 | 119.3 |
| P2—Pt1—Cl1 | 90.20 (9) | C14—C19—C18 | 116.7 (10) |
| P1—Pt1—Cl2 | 88.05 (10) | C14—C19—C20 | 121.1 (10) |
| P2—Pt1—Cl2 | 177.30 (9) | C18—C19—C20 | 122.2 (10) |
| Cl1—Pt1—Cl2 | 88.47 (10) | C16—C17—C18 | 120.4 (11) |
| O2—P1—O1 | 105.7 (4) | C16—C17—H17 | 119.8 |
| O2—P1—C12 | 100.9 (5) | C18—C17—H17 | 119.8 |
| O1—P1—C12 | 102.7 (5) | C17—C16—C15 | 120.4 (11) |
| O2—P1—Pt1 | 115.3 (3) | C17—C16—H16 | 119.8 |
| O1—P1—Pt1 | 110.6 (3) | C15—C16—H16 | 119.8 |
| C12—P1—Pt1 | 120.0 (4) | C16—C15—C14 | 118.3 (11) |
| O4—P2—O3 | 103.9 (4) | C16—C15—H15 | 120.8 |
| O4—P2—C25 | 102.2 (5) | C14—C15—H15 | 120.8 |
| O3—P2—C25 | 103.7 (4) | C19—C14—C15 | 122.8 (10) |
| O4—P2—Pt1 | 117.8 (3) | C19—C14—O3 | 121.1 (9) |
| O3—P2—Pt1 | 112.8 (3) | C15—C14—O3 | 116.1 (9) |
| C25—P2—Pt1 | 114.8 (4) | C24—C25—C20 | 122.5 (9) |
| C13—O2—P1 | 121.6 (8) | C24—C25—P2 | 120.7 (8) |
| C1—O1—P1 | 120.7 (6) | C20—C25—P2 | 116.4 (8) |
| C26—O4—P2 | 119.8 (7) | C25—C24—C23 | 119.0 (10) |
| C14—O3—P2 | 116.7 (6) | C25—C24—H24 | 120.5 |
| C9—C8—C7 | 121.3 (12) | C23—C24—H24 | 120.5 |
| C9—C8—H8 | 119.4 | C22—C23—C24 | 119.6 (11) |
| C7—C8—H8 | 119.4 | C22—C23—H23 | 120.2 |
| C21—C20—C25 | 116.9 (10) | C24—C23—H23 | 120.2 |
| C21—C20—C19 | 122.0 (10) | C23—C22—C21 | 121.4 (11) |
| C25—C20—C19 | 121.2 (9) | C23—C22—H22 | 119.3 |
| C4—C5—C6 | 122.8 (11) | C21—C22—H22 | 119.3 |
| C4—C5—H5 | 118.6 | C8—C7—C12 | 117.8 (11) |
| C6—C5—H5 | 118.6 | C8—C7—C6 | 121.9 (11) |
| C1—C6—C5 | 114.8 (10) | C12—C7—C6 | 120.3 (10) |
| C1—C6—C7 | 122.2 (10) | O2—C13—H13A | 109.5 |
| C5—C6—C7 | 122.9 (10) | O2—C13—H13B | 109.5 |
| C5—C4—C3 | 121.2 (10) | H13A—C13—H13B | 109.5 |
| C5—C4—H4 | 119.4 | O2—C13—H13C | 109.5 |
| C3—C4—H4 | 119.4 | H13A—C13—H13C | 109.5 |
| C4—C3—C2 | 119.3 (11) | H13B—C13—H13C | 109.5 |
| C4—C3—H3 | 120.3 | C22—C21—C20 | 120.6 (11) |
| C2—C3—H3 | 120.3 | C22—C21—H21 | 119.7 |
| C3—C2—C1 | 118.0 (10) | C20—C21—H21 | 119.7 |
| C3—C2—H2 | 121.0 | O4—C26—H26A | 109.5 |
| C1—C2—H2 | 121.0 | O4—C26—H26B | 109.5 |
| O1—C1—C6 | 121.4 (9) | H26A—C26—H26B | 109.5 |
| O1—C1—C2 | 114.8 (9) | O4—C26—H26C | 109.5 |
| C6—C1—C2 | 123.8 (10) | H26A—C26—H26C | 109.5 |
| C7—C12—C11 | 121.1 (10) | H26B—C26—H26C | 109.5 |
| C7—C12—P1 | 119.5 (8) | Cl4A—C27—Cl5A | 116.8 (7) |
| C11—C12—P1 | 119.4 (9) | Cl4B—C27—Cl5B | 111.4 (8) |
| C10—C11—C12 | 119.5 (11) | Cl4A—C27—Cl3A | 109.2 (6) |
| C10—C11—H11 | 120.2 | Cl5A—C27—Cl3A | 108.1 (5) |
| C12—C11—H11 | 120.2 | Cl4B—C27—Cl3B | 106.4 (7) |
| C9—C10—C11 | 119.1 (11) | Cl5B—C27—Cl3B | 103.9 (7) |
| C9—C10—H10 | 120.4 | Cl4A—C27—H27 | 109.4 |
| C11—C10—H10 | 120.4 | Cl5A—C27—H27 | 106.7 |
| C8—C9—C10 | 121.2 (12) | Cl4B—C27—H27 | 122.5 |
| C8—C9—H9 | 119.4 | Cl5B—C27—H27 | 96.6 |
| C10—C9—H9 | 119.4 | Cl3A—C27—H27 | 105.9 |
| C17—C18—C19 | 121.4 (10) | Cl3B—C27—H27 | 114.2 |
| | | |
| Cl1—Pt1—P2—O4 | −10.8 (3) | C25—C20—C19—C14 | −24.2 (15) |
| Cl2—Pt1—P1—O2 | −44.1 (4) | O1—P1—Pt1—P2 | 13.7 (3) |
| C12—C7—C6—C1 | −13.9 (16) | O3—P2—Pt1—P1 | 49.8 (3) |
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| C27—H27···Cl1i | 0.97 | 2.59 | 3.491 (14) | 154 |
| C27—H27···O4i | 0.97 | 2.57 | 3.226 (17) | 125 |
| Symmetry codes: (i) −x+1, −y, −z+1. |
Table 1
Selected geometric parameters (Å) top| Pt1—P1 | 2.188 (3) | Pt1—Cl1 | 2.325 (3) |
| Pt1—P2 | 2.201 (3) | Pt1—Cl2 | 2.351 (3) |
Table 2
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| C27—H27···Cl1i | 0.97 | 2.59 | 3.491 (14) | 154 |
| C27—H27···O4i | 0.97 | 2.57 | 3.226 (17) | 125 |
| Symmetry codes: (i) −x+1, −y, −z+1. |
TH thanks the HAS CRC for financial support and also a computer purchase
administered through OTKA grant No. T-049712 kindly provided by Professor A.
Kálmán. The authors are also grateful for partial funding from OTKA grants
T-067679 (AK and GyK) and T-75869 (MC and TH).
Allen, F. H. (2002). Acta Cryst. B58, 380–388.
Claver, C., Fernandez, E., Gillon, A. L., Heslop, K. M., Hyett, D. J., Martorell, A., Orpen, A. G. & Pringle, P. G. (2000). Chem. Commun. pp. 961–962.
Keglevich, Gy., Kerényi, A., Mayer, B., Körtvélyesi, T. & Ludányi, K. (2008). Transition Met. Chem. 33, 505–510.
Rigaku (2008). CrystalStructure. Rigaku Corporation, The Woodlands, Texas, USA.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
Spek, A. L. (2009). Acta Cryst. D65, 148–155.
Syntheses, spectroscopic data and theoretical chemistry modeling of various dibenzooxaphosphorines including the parent compound of the title solvate have been reported by Keglevich et al. (2008).
The asymmetric unit of the title compound is shown in Fig. 1. The structure of the complex in the crystalline state is in agreement with that reported from theoretical modeling. A more stable cis form is prefered over the trans, with a syn-periplanar disposition of O—P—Pt—P torsion angles (O1—P1—Pt1—P2 ca 13.7 (3)° and O3—P2—Pt1—P1 ca 49.8 (3)°). However, Pt—P and Pt—-Cl distances appear to be 0.05–0.1 Å shorter in the crystal structure, compared to a theoretical model.
The shortest ring center···center distance of 3.658 (8) Å is observed between C14-C19 benzene rings of complex molecules at (x, y, z) and (1 -x, - y, 2 - z). The only other crystal structure in the CSD (Allen, 2002) having P—Pt—P bridging is MARJEU from the Orpen group (Claver et al., 2000). MARJEU entraps two kinds of solvents in differing stoichiometric ratios (1 for THF and 0.76 for dichloromethane) in its crystal. The title compound also shows disorder of the solvent placed near to inversion centres at (1/2, 1/2, 0) in channels parallel to the a axis. Partial fixation of the solvent occurs via bifurcated C—H ··· O and C—H ··· Cl close contacts from the trichloromethane H atom to an alkoxy O4 atom and to Cl1 (Table 2). Electronic influences of these interactions may also be reflected in the unequal bonding geometry around the metal center. Existence of this C—H···X interaction seems to be also corroborated by IR investigations that will be reported elsewhere together with the room-temperature X-ray study of this compound. It appears from these results that the trichloromethane guest disorder is partly of kinetical nature. The C and H atom positions are relatively well kept while chlorine atoms change their positions with respect to the C—H bond.