Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807032254/cv2263sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807032254/cv2263Isup2.hkl |
CCDC reference: 657550
Key indicators
- Single-crystal X-ray study
- T = 283 K
- Mean (C-C) = 0.005 Å
- R factor = 0.020
- wR factor = 0.045
- Data-to-parameter ratio = 22.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.54 Ratio
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.95 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.54 PLAT230_ALERT_2_C Hirshfeld Test Diff for C31 - C32 .. 5.24 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn - C3 .. 6.15 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn - C4 .. 7.23 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C49 PLAT320_ALERT_2_C Check Hybridisation of C1 in Main Residue . ? PLAT320_ALERT_2_C Check Hybridisation of C3 in Main Residue . ? PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C1 - C2 ... 1.33 Ang.
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 9675 Count of symmetry unique reflns 5384 Completeness (_total/calc) 179.70% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 4291 Fraction of Friedel pairs measured 0.797 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 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 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Corresponding geometry in the related MnPt complex with the chelating bis(diphenylphosphino)methane ligand was reported by Dolgushin et al. (2001). For crystal structures of related µ-carbene complexes containing the Mn—Pt-µ-C triangle system, see: Jeffery et al. (1981). For details of the synthesis, see: Antonova et al. (1985).
The title compound was prepared by the interaction between Cp(CO)2Mn?C? CHPh and Pt(PPh3)4 (diethyl ether, 298 K, 1 h) (Antonova et al., 1985). Suitable single crystals were obtained by isothermal evaporation of an ether solution at 298 K.
Seven phenyl rings of the title molecule were idealized and refined as rigid groups with C—C bond lengths of 1.390 Å. All H atoms were positioned geometrically (C—H 0.93 Å) and refined using a riding model with Uiso(H) = 1.2 Ueq(C).
The molecule of the title compound, (I), is the dinuclear complex containing the Mn and Pt atoms bridged by the µ-phenylvinylidene ligand and semi-bridged by carbonyl group. The phenyl ring and the C?C bond of vinylidene coupling with the Mn—Pt-µ-C triangle form an almost planar system. Corresponding geometry was found for the related MnPt complex with chelating bis(diphenylphosphino)methane at the Pt atom (Dolgushin et al., 2001). The structures of some µ-carbene complexes containing the Mn—Pt-µ-C triangle system as a molecular central fragment were reported (Jeffery et al., 1981).
Corresponding geometry in the related MnPt complex with the chelating bis(diphenylphosphino)methane ligand was reported by Dolgushin et al. (2001). For crystal structures of related µ-carbene complexes containing the Mn—Pt-µ-C triangle system, see: Jeffery et al. (1981). For details of the synthesis, see: Antonova et al. (1985).
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. The molecular structure of the title compound with atomic labels and 50% probability displacement ellipsoids. All H-atoms, except H2, omitted for clarity. |
[MnPt(C5H5)(C8H6)(C18H15P)2(CO)2] | F(000) = 1984 |
Mr = 997.81 | Dx = 1.569 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 9978 reflections |
a = 11.1320 (4) Å | θ = 2.4–27.5° |
b = 19.4463 (7) Å | µ = 3.72 mm−1 |
c = 19.5174 (7) Å | T = 283 K |
V = 4225.1 (3) Å3 | Block, red |
Z = 4 | 0.29 × 0.17 × 0.14 mm |
Bruker SMART 4K CCD area-detector diffractometer | 9675 independent reflections |
Radiation source: sealed tube | 8974 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
φ and ω scans | θmax = 27.5°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | h = −14→14 |
Tmin = 0.352, Tmax = 0.624 | k = −25→25 |
37385 measured reflections | l = −25→25 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: constr |
R[F2 > 2σ(F2)] = 0.020 | H-atom parameters constrained |
wR(F2) = 0.045 | w = 1/[σ2(Fo2) + (0.0241P)2 + 2.8014P] where P = (Fo2 + 2Fc2)/3 |
S = 0.95 | (Δ/σ)max = 0.011 |
9675 reflections | Δρmax = 0.63 e Å−3 |
433 parameters | Δρmin = −0.25 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 4291 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.007 (3) |
[MnPt(C5H5)(C8H6)(C18H15P)2(CO)2] | V = 4225.1 (3) Å3 |
Mr = 997.81 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 11.1320 (4) Å | µ = 3.72 mm−1 |
b = 19.4463 (7) Å | T = 283 K |
c = 19.5174 (7) Å | 0.29 × 0.17 × 0.14 mm |
Bruker SMART 4K CCD area-detector diffractometer | 9675 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | 8974 reflections with I > 2σ(I) |
Tmin = 0.352, Tmax = 0.624 | Rint = 0.026 |
37385 measured reflections |
R[F2 > 2σ(F2)] = 0.020 | H-atom parameters constrained |
wR(F2) = 0.045 | Δρmax = 0.63 e Å−3 |
S = 0.95 | Δρmin = −0.25 e Å−3 |
9675 reflections | Absolute structure: Flack (1983), 4291 Friedel pairs |
433 parameters | Absolute structure parameter: −0.007 (3) |
0 restraints |
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 | ||
Pt | 0.442096 (9) | 0.414461 (5) | 0.378591 (5) | 0.03419 (3) | |
Mn | 0.22734 (4) | 0.46992 (2) | 0.36592 (2) | 0.03741 (10) | |
C3 | 0.2363 (3) | 0.37832 (16) | 0.38176 (18) | 0.0476 (7) | |
O3 | 0.2169 (2) | 0.32086 (12) | 0.39299 (14) | 0.0623 (7) | |
C4 | 0.1687 (3) | 0.47710 (18) | 0.44942 (19) | 0.0527 (8) | |
O4 | 0.1316 (3) | 0.48242 (15) | 0.50469 (14) | 0.0829 (9) | |
C11 | 0.0687 (3) | 0.48385 (18) | 0.30666 (18) | 0.0572 (9) | |
H11 | −0.0055 | 0.4656 | 0.3190 | 0.069* | |
C12 | 0.1152 (3) | 0.54915 (18) | 0.32649 (17) | 0.0523 (8) | |
H12 | 0.0768 | 0.5811 | 0.3543 | 0.063* | |
C13 | 0.2283 (3) | 0.55672 (17) | 0.29704 (16) | 0.0465 (7) | |
H13 | 0.2784 | 0.5947 | 0.3015 | 0.056* | |
C14 | 0.2538 (3) | 0.49653 (17) | 0.25917 (15) | 0.0476 (7) | |
H14 | 0.3236 | 0.4877 | 0.2345 | 0.057* | |
C15 | 0.1545 (3) | 0.45249 (17) | 0.26547 (17) | 0.0535 (9) | |
H15 | 0.1473 | 0.4093 | 0.2454 | 0.064* | |
C1 | 0.3757 (2) | 0.50564 (15) | 0.40819 (14) | 0.0367 (6) | |
C2 | 0.4220 (3) | 0.56321 (15) | 0.43342 (16) | 0.0451 (7) | |
H2 | 0.4997 | 0.5584 | 0.4502 | 0.054* | |
C5 | 0.37250 (19) | 0.63388 (8) | 0.43978 (11) | 0.0466 (7) | |
C6 | 0.45344 (16) | 0.68831 (12) | 0.43990 (13) | 0.0639 (9) | |
H6 | 0.5355 | 0.6797 | 0.4372 | 0.077* | |
C7 | 0.4117 (2) | 0.75556 (10) | 0.44408 (13) | 0.0756 (12) | |
H7 | 0.4659 | 0.7920 | 0.4442 | 0.091* | |
C8 | 0.2891 (3) | 0.76837 (8) | 0.44814 (13) | 0.0763 (13) | |
H8 | 0.2612 | 0.8134 | 0.4509 | 0.092* | |
C9 | 0.20817 (18) | 0.71395 (12) | 0.44802 (12) | 0.0665 (11) | |
H9 | 0.1261 | 0.7225 | 0.4507 | 0.080* | |
C10 | 0.24987 (17) | 0.64670 (10) | 0.44383 (11) | 0.0509 (8) | |
H10 | 0.1957 | 0.6103 | 0.4438 | 0.061* | |
P1 | 0.61667 (6) | 0.41618 (4) | 0.43912 (3) | 0.03333 (14) | |
C16 | 0.58867 (16) | 0.41181 (11) | 0.53218 (7) | 0.0375 (6) | |
C17 | 0.67643 (14) | 0.38760 (11) | 0.57673 (10) | 0.0492 (8) | |
H17 | 0.7493 | 0.3718 | 0.5596 | 0.059* | |
C18 | 0.65531 (19) | 0.38708 (12) | 0.64692 (9) | 0.0590 (9) | |
H18 | 0.7140 | 0.3709 | 0.6767 | 0.071* | |
C19 | 0.5464 (2) | 0.41076 (13) | 0.67256 (7) | 0.0680 (10) | |
H19 | 0.5323 | 0.4104 | 0.7195 | 0.082* | |
C20 | 0.45865 (17) | 0.43497 (12) | 0.62802 (10) | 0.0678 (10) | |
H20 | 0.3858 | 0.4508 | 0.6452 | 0.081* | |
C21 | 0.47977 (15) | 0.43550 (11) | 0.55783 (10) | 0.0505 (8) | |
H21 | 0.4210 | 0.4517 | 0.5280 | 0.061* | |
C22 | 0.73105 (14) | 0.34921 (8) | 0.42635 (11) | 0.0349 (6) | |
C23 | 0.71731 (16) | 0.28461 (10) | 0.45581 (10) | 0.0481 (8) | |
H23 | 0.6498 | 0.2750 | 0.4822 | 0.058* | |
C24 | 0.8044 (2) | 0.23441 (8) | 0.44583 (12) | 0.0587 (9) | |
H24 | 0.7953 | 0.1912 | 0.4655 | 0.070* | |
C25 | 0.90533 (17) | 0.24880 (10) | 0.40639 (12) | 0.0617 (10) | |
H25 | 0.9636 | 0.2152 | 0.3997 | 0.074* | |
C26 | 0.91907 (14) | 0.31340 (11) | 0.37693 (12) | 0.0617 (9) | |
H26 | 0.9866 | 0.3230 | 0.3505 | 0.074* | |
C27 | 0.83193 (17) | 0.36360 (8) | 0.38691 (11) | 0.0512 (8) | |
H27 | 0.8411 | 0.4068 | 0.3672 | 0.061* | |
C28 | 0.70882 (17) | 0.49435 (9) | 0.42915 (11) | 0.0394 (7) | |
C29 | 0.7922 (2) | 0.51345 (10) | 0.47865 (10) | 0.0567 (9) | |
H29 | 0.8022 | 0.4867 | 0.5177 | 0.068* | |
C30 | 0.86057 (18) | 0.57258 (11) | 0.46976 (12) | 0.0675 (11) | |
H30 | 0.9163 | 0.5854 | 0.5029 | 0.081* | |
C31 | 0.8456 (2) | 0.61260 (9) | 0.41137 (13) | 0.0636 (10) | |
H31 | 0.8914 | 0.6522 | 0.4054 | 0.076* | |
C32 | 0.7623 (2) | 0.59349 (10) | 0.36187 (10) | 0.0669 (10) | |
H32 | 0.7523 | 0.6203 | 0.3228 | 0.080* | |
C33 | 0.69389 (18) | 0.53437 (11) | 0.37076 (10) | 0.0524 (8) | |
H33 | 0.6381 | 0.5216 | 0.3376 | 0.063* | |
P2 | 0.47665 (7) | 0.32551 (4) | 0.29914 (4) | 0.03942 (18) | |
C34 | 0.36562 (19) | 0.32082 (12) | 0.22906 (10) | 0.0497 (8) | |
C35 | 0.2647 (2) | 0.27973 (11) | 0.23820 (12) | 0.0650 (11) | |
H35 | 0.2570 | 0.2532 | 0.2776 | 0.078* | |
C36 | 0.1754 (2) | 0.27830 (14) | 0.18846 (17) | 0.0879 (15) | |
H36 | 0.1079 | 0.2508 | 0.1946 | 0.105* | |
C37 | 0.1870 (3) | 0.31797 (17) | 0.12958 (14) | 0.107 (2) | |
H37 | 0.1272 | 0.3170 | 0.0963 | 0.128* | |
C38 | 0.2879 (3) | 0.35906 (15) | 0.12044 (10) | 0.0996 (16) | |
H38 | 0.2956 | 0.3856 | 0.0810 | 0.120* | |
C39 | 0.3772 (2) | 0.36048 (12) | 0.17018 (12) | 0.0717 (11) | |
H39 | 0.4447 | 0.3880 | 0.1641 | 0.086* | |
C40 | 0.48294 (18) | 0.23474 (8) | 0.32309 (10) | 0.0408 (7) | |
C41 | 0.4953 (2) | 0.18370 (11) | 0.27372 (8) | 0.0534 (8) | |
H41 | 0.4983 | 0.1954 | 0.2276 | 0.064* | |
C42 | 0.5033 (2) | 0.11515 (9) | 0.29336 (12) | 0.0644 (10) | |
H42 | 0.5116 | 0.0810 | 0.2603 | 0.077* | |
C43 | 0.4989 (2) | 0.09763 (8) | 0.36236 (14) | 0.0696 (11) | |
H43 | 0.5042 | 0.0518 | 0.3755 | 0.083* | |
C44 | 0.4865 (2) | 0.14866 (12) | 0.41172 (9) | 0.0654 (10) | |
H44 | 0.4835 | 0.1369 | 0.4579 | 0.079* | |
C45 | 0.47853 (19) | 0.21722 (10) | 0.39209 (9) | 0.0514 (8) | |
H45 | 0.4702 | 0.2514 | 0.4251 | 0.062* | |
C46 | 0.61840 (18) | 0.34361 (13) | 0.25456 (11) | 0.0539 (9) | |
C47 | 0.6366 (3) | 0.41109 (12) | 0.23350 (14) | 0.0776 (12) | |
H47 | 0.5772 | 0.4439 | 0.2408 | 0.093* | |
C48 | 0.7435 (3) | 0.42947 (15) | 0.20160 (15) | 0.112 (2) | |
H48 | 0.7557 | 0.4746 | 0.1875 | 0.134* | |
C49 | 0.8322 (2) | 0.3804 (2) | 0.19075 (15) | 0.124 (3) | |
H49 | 0.9038 | 0.3927 | 0.1694 | 0.149* | |
C50 | 0.8140 (2) | 0.31289 (19) | 0.21181 (15) | 0.1025 (18) | |
H50 | 0.8734 | 0.2800 | 0.2046 | 0.123* | |
C51 | 0.7071 (2) | 0.29451 (12) | 0.24372 (13) | 0.0691 (11) | |
H51 | 0.6950 | 0.2494 | 0.2578 | 0.083* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt | 0.02976 (5) | 0.03379 (5) | 0.03903 (5) | 0.00328 (4) | −0.00323 (5) | −0.00160 (5) |
Mn | 0.0300 (2) | 0.0391 (2) | 0.0431 (3) | 0.00275 (17) | −0.00165 (19) | 0.0078 (2) |
C3 | 0.0390 (15) | 0.0498 (18) | 0.0541 (19) | −0.0004 (13) | −0.0131 (16) | 0.0089 (17) |
O3 | 0.0487 (13) | 0.0455 (13) | 0.093 (2) | −0.0087 (10) | −0.0133 (13) | 0.0173 (13) |
C4 | 0.0438 (18) | 0.055 (2) | 0.059 (2) | 0.0040 (16) | 0.0026 (17) | 0.0154 (17) |
O4 | 0.090 (2) | 0.097 (2) | 0.0622 (17) | 0.0087 (17) | 0.0326 (16) | 0.0184 (15) |
C11 | 0.0343 (17) | 0.069 (2) | 0.068 (2) | −0.0031 (18) | −0.0116 (18) | 0.0224 (18) |
C12 | 0.0473 (18) | 0.057 (2) | 0.053 (2) | 0.0162 (16) | −0.0060 (15) | 0.0099 (16) |
C13 | 0.0469 (18) | 0.0446 (17) | 0.0480 (18) | 0.0006 (14) | −0.0064 (15) | 0.0105 (14) |
C14 | 0.0517 (19) | 0.054 (2) | 0.0376 (16) | 0.0057 (16) | −0.0038 (14) | 0.0048 (14) |
C15 | 0.059 (2) | 0.0473 (19) | 0.054 (2) | −0.0007 (16) | −0.0217 (17) | 0.0066 (15) |
C1 | 0.0316 (14) | 0.0388 (16) | 0.0396 (15) | 0.0069 (12) | 0.0003 (12) | −0.0027 (12) |
C2 | 0.0403 (17) | 0.0436 (16) | 0.0514 (17) | 0.0076 (13) | −0.0065 (14) | −0.0063 (13) |
C5 | 0.056 (2) | 0.0446 (18) | 0.0386 (17) | 0.0059 (15) | −0.0002 (14) | −0.0043 (14) |
C6 | 0.072 (3) | 0.051 (2) | 0.068 (2) | −0.010 (2) | 0.005 (2) | −0.0109 (17) |
C7 | 0.106 (3) | 0.041 (2) | 0.080 (3) | −0.008 (2) | 0.003 (2) | −0.0045 (19) |
C8 | 0.120 (4) | 0.043 (2) | 0.066 (3) | 0.017 (2) | −0.013 (3) | −0.0073 (18) |
C9 | 0.080 (3) | 0.061 (2) | 0.058 (2) | 0.027 (2) | −0.010 (2) | −0.0063 (18) |
C10 | 0.059 (2) | 0.0469 (19) | 0.0462 (19) | 0.0103 (16) | −0.0040 (15) | −0.0026 (15) |
P1 | 0.0283 (3) | 0.0347 (3) | 0.0370 (4) | 0.0017 (3) | −0.0003 (3) | −0.0014 (3) |
C16 | 0.0362 (14) | 0.0360 (14) | 0.0403 (14) | −0.0019 (13) | 0.0017 (11) | −0.0037 (14) |
C17 | 0.0465 (18) | 0.057 (2) | 0.0438 (18) | 0.0013 (15) | −0.0061 (14) | −0.0044 (14) |
C18 | 0.076 (2) | 0.058 (2) | 0.0427 (18) | −0.0018 (18) | −0.0076 (17) | −0.0030 (15) |
C19 | 0.100 (3) | 0.068 (2) | 0.0370 (16) | −0.004 (3) | 0.0128 (19) | −0.0091 (17) |
C20 | 0.074 (2) | 0.074 (2) | 0.056 (2) | 0.0110 (19) | 0.023 (2) | −0.0104 (18) |
C21 | 0.0527 (19) | 0.0512 (19) | 0.0475 (18) | 0.0101 (15) | 0.0081 (15) | −0.0024 (14) |
C22 | 0.0291 (14) | 0.0395 (16) | 0.0363 (15) | 0.0046 (12) | −0.0008 (11) | −0.0031 (12) |
C23 | 0.0418 (18) | 0.0488 (19) | 0.054 (2) | 0.0067 (14) | 0.0009 (15) | 0.0010 (15) |
C24 | 0.067 (2) | 0.0404 (18) | 0.069 (2) | 0.0173 (17) | −0.0057 (19) | −0.0005 (16) |
C25 | 0.053 (2) | 0.059 (2) | 0.073 (2) | 0.0256 (17) | −0.0055 (17) | −0.0111 (19) |
C26 | 0.0396 (17) | 0.071 (2) | 0.075 (2) | 0.0102 (15) | 0.0130 (18) | −0.010 (2) |
C27 | 0.0396 (16) | 0.0487 (17) | 0.065 (2) | 0.0065 (13) | 0.0086 (17) | 0.0031 (17) |
C28 | 0.0326 (15) | 0.0343 (15) | 0.0513 (18) | 0.0027 (12) | 0.0053 (13) | −0.0041 (13) |
C29 | 0.055 (2) | 0.0459 (19) | 0.069 (2) | −0.0013 (16) | −0.0159 (17) | 0.0033 (17) |
C30 | 0.056 (2) | 0.041 (2) | 0.106 (3) | −0.0062 (16) | −0.017 (2) | −0.0147 (19) |
C31 | 0.055 (2) | 0.0401 (18) | 0.095 (3) | −0.0094 (16) | 0.014 (2) | −0.0115 (19) |
C32 | 0.081 (2) | 0.050 (2) | 0.070 (2) | −0.0014 (19) | 0.019 (2) | 0.0101 (19) |
C33 | 0.0588 (19) | 0.0487 (17) | 0.0497 (19) | −0.0058 (15) | 0.0030 (17) | 0.0020 (16) |
P2 | 0.0405 (4) | 0.0372 (4) | 0.0406 (4) | 0.0017 (3) | −0.0012 (3) | −0.0043 (3) |
C34 | 0.062 (2) | 0.0414 (18) | 0.0456 (18) | 0.0124 (16) | −0.0118 (16) | −0.0120 (14) |
C35 | 0.062 (2) | 0.046 (2) | 0.088 (3) | 0.0081 (17) | −0.028 (2) | −0.0165 (19) |
C36 | 0.078 (3) | 0.065 (3) | 0.121 (4) | 0.014 (2) | −0.047 (3) | −0.040 (3) |
C37 | 0.125 (4) | 0.111 (4) | 0.084 (4) | 0.050 (3) | −0.063 (3) | −0.050 (3) |
C38 | 0.143 (5) | 0.111 (4) | 0.044 (2) | 0.042 (3) | −0.025 (3) | −0.007 (3) |
C39 | 0.091 (3) | 0.079 (3) | 0.045 (2) | 0.018 (2) | −0.006 (2) | −0.0082 (19) |
C40 | 0.0361 (15) | 0.0367 (16) | 0.0498 (17) | 0.0043 (12) | −0.0015 (12) | −0.0017 (13) |
C41 | 0.0520 (19) | 0.0454 (19) | 0.063 (2) | 0.0126 (15) | 0.0006 (17) | −0.0043 (16) |
C42 | 0.056 (2) | 0.045 (2) | 0.092 (3) | 0.0104 (17) | −0.003 (2) | −0.0141 (19) |
C43 | 0.060 (2) | 0.044 (2) | 0.104 (3) | 0.0073 (16) | 0.000 (2) | 0.015 (2) |
C44 | 0.055 (2) | 0.069 (3) | 0.072 (2) | −0.0015 (18) | −0.0058 (18) | 0.020 (2) |
C45 | 0.0461 (17) | 0.0490 (18) | 0.059 (2) | 0.0055 (13) | −0.0013 (15) | 0.0006 (15) |
C46 | 0.055 (2) | 0.066 (2) | 0.0409 (18) | −0.0111 (18) | 0.0037 (16) | −0.0115 (16) |
C47 | 0.094 (3) | 0.075 (3) | 0.063 (2) | −0.031 (3) | 0.013 (2) | −0.004 (2) |
C48 | 0.137 (5) | 0.121 (5) | 0.076 (3) | −0.074 (4) | 0.035 (3) | −0.009 (3) |
C49 | 0.096 (4) | 0.199 (7) | 0.076 (3) | −0.075 (4) | 0.030 (3) | −0.046 (4) |
C50 | 0.056 (3) | 0.168 (5) | 0.083 (3) | −0.017 (3) | 0.019 (2) | −0.045 (3) |
C51 | 0.051 (2) | 0.092 (3) | 0.064 (2) | −0.005 (2) | 0.0084 (18) | −0.017 (2) |
Pt—C1 | 2.006 (3) | C23—H23 | 0.9300 |
Pt—C3 | 2.397 (3) | C24—C25 | 1.3900 |
Pt—P1 | 2.2745 (7) | C24—H24 | 0.9300 |
Pt—P2 | 2.3548 (8) | C25—C26 | 1.3900 |
Pt—Mn | 2.6344 (4) | C25—H25 | 0.9300 |
Mn—C1 | 1.972 (3) | C26—C27 | 1.3900 |
Mn—C3 | 1.811 (3) | C26—H26 | 0.9300 |
Mn—C4 | 1.761 (4) | C27—H27 | 0.9300 |
Mn—C11 | 2.129 (3) | C28—C29 | 1.3900 |
Mn—C12 | 2.127 (3) | C28—C33 | 1.3900 |
Mn—C13 | 2.158 (3) | C29—C30 | 1.3900 |
Mn—C14 | 2.167 (3) | C29—H29 | 0.9300 |
Mn—C15 | 2.149 (3) | C30—C31 | 1.3900 |
C3—O3 | 1.159 (3) | C30—H30 | 0.9300 |
C4—O4 | 1.160 (4) | C31—C32 | 1.3900 |
C11—C15 | 1.390 (5) | C31—H31 | 0.9300 |
C11—C12 | 1.425 (5) | C32—C33 | 1.3900 |
C11—H11 | 0.9300 | C32—H32 | 0.9300 |
C12—C13 | 1.391 (5) | C33—H33 | 0.9300 |
C12—H12 | 0.9300 | P2—C40 | 1.8273 (16) |
C13—C14 | 1.413 (4) | P2—C46 | 1.8359 (19) |
C13—H13 | 0.9300 | P2—C34 | 1.8457 (18) |
C14—C15 | 1.404 (5) | C34—C35 | 1.3900 |
C14—H14 | 0.9300 | C34—C39 | 1.3900 |
C15—H15 | 0.9300 | C35—C36 | 1.3900 |
C1—C2 | 1.327 (4) | C35—H35 | 0.9300 |
C2—C5 | 1.486 (3) | C36—C37 | 1.3900 |
C2—H2 | 0.9300 | C36—H36 | 0.9300 |
C5—C6 | 1.3900 | C37—C38 | 1.3900 |
C5—C10 | 1.3900 | C37—H37 | 0.9300 |
C6—C7 | 1.3900 | C38—C39 | 1.3900 |
C6—H6 | 0.9300 | C38—H38 | 0.9300 |
C7—C8 | 1.3900 | C39—H39 | 0.9300 |
C7—H7 | 0.9300 | C40—C41 | 1.3900 |
C8—C9 | 1.3900 | C40—C45 | 1.3900 |
C8—H8 | 0.9300 | C41—C42 | 1.3900 |
C9—C10 | 1.3900 | C41—H41 | 0.9300 |
C9—H9 | 0.9300 | C42—C43 | 1.3900 |
C10—H10 | 0.9300 | C42—H42 | 0.9300 |
P1—C22 | 1.8382 (15) | C43—C44 | 1.3900 |
P1—C28 | 1.8442 (16) | C43—H43 | 0.9300 |
P1—C16 | 1.8448 (15) | C44—C45 | 1.3900 |
C16—C17 | 1.3900 | C44—H44 | 0.9300 |
C16—C21 | 1.3900 | C45—H45 | 0.9300 |
C17—C18 | 1.3900 | C46—C47 | 1.3900 |
C17—H17 | 0.9300 | C46—C51 | 1.3900 |
C18—C19 | 1.3900 | C47—C48 | 1.3900 |
C18—H18 | 0.9300 | C47—H47 | 0.9300 |
C19—C20 | 1.3900 | C48—C49 | 1.3900 |
C19—H19 | 0.9300 | C48—H48 | 0.9300 |
C20—C21 | 1.3900 | C49—C50 | 1.3900 |
C20—H20 | 0.9300 | C49—H49 | 0.9300 |
C21—H21 | 0.9300 | C50—C51 | 1.3900 |
C22—C23 | 1.3900 | C50—H50 | 0.9300 |
C22—C27 | 1.3900 | C51—H51 | 0.9300 |
C23—C24 | 1.3900 | ||
C1—Pt—P1 | 98.76 (8) | C21—C16—P1 | 119.12 (11) |
C1—Pt—P2 | 154.04 (8) | C16—C17—C18 | 120.0 |
P1—Pt—P2 | 102.31 (3) | C16—C17—H17 | 120.0 |
C1—Pt—C3 | 84.23 (11) | C18—C17—H17 | 120.0 |
P1—Pt—C3 | 143.85 (8) | C19—C18—C17 | 120.0 |
P2—Pt—C3 | 87.58 (8) | C19—C18—H18 | 120.0 |
C1—Pt—Mn | 47.99 (8) | C17—C18—H18 | 120.0 |
P1—Pt—Mn | 144.90 (2) | C20—C19—C18 | 120.0 |
P2—Pt—Mn | 112.78 (2) | C20—C19—H19 | 120.0 |
C3—Pt—Mn | 41.86 (7) | C18—C19—H19 | 120.0 |
C4—Mn—C3 | 86.59 (16) | C21—C20—C19 | 120.0 |
C4—Mn—C1 | 84.00 (14) | C21—C20—H20 | 120.0 |
C3—Mn—C1 | 103.22 (13) | C19—C20—H20 | 120.0 |
C4—Mn—C12 | 93.44 (14) | C20—C21—C16 | 120.0 |
C3—Mn—C12 | 143.79 (13) | C20—C21—H21 | 120.0 |
C1—Mn—C12 | 112.80 (13) | C16—C21—H21 | 120.0 |
C4—Mn—C11 | 100.66 (15) | C23—C22—C27 | 120.0 |
C3—Mn—C11 | 105.29 (14) | C23—C22—P1 | 120.53 (11) |
C1—Mn—C11 | 151.32 (13) | C27—C22—P1 | 119.47 (11) |
C12—Mn—C11 | 39.13 (13) | C22—C23—C24 | 120.0 |
C4—Mn—C15 | 135.80 (15) | C22—C23—H23 | 120.0 |
C3—Mn—C15 | 91.22 (14) | C24—C23—H23 | 120.0 |
C1—Mn—C15 | 138.88 (13) | C25—C24—C23 | 120.0 |
C12—Mn—C15 | 64.06 (13) | C25—C24—H24 | 120.0 |
C11—Mn—C15 | 37.91 (13) | C23—C24—H24 | 120.0 |
C4—Mn—C13 | 121.09 (14) | C24—C25—C26 | 120.0 |
C3—Mn—C13 | 151.11 (15) | C24—C25—H25 | 120.0 |
C1—Mn—C13 | 88.91 (12) | C26—C25—H25 | 120.0 |
C12—Mn—C13 | 37.89 (12) | C25—C26—C27 | 120.0 |
C11—Mn—C13 | 64.29 (12) | C25—C26—H26 | 120.0 |
C15—Mn—C13 | 63.70 (12) | C27—C26—H26 | 120.0 |
C4—Mn—C14 | 157.10 (14) | C26—C27—C22 | 120.0 |
C3—Mn—C14 | 113.05 (15) | C26—C27—H27 | 120.0 |
C1—Mn—C14 | 101.79 (12) | C22—C27—H27 | 120.0 |
C12—Mn—C14 | 63.82 (13) | C29—C28—C33 | 120.0 |
C11—Mn—C14 | 63.89 (13) | C29—C28—P1 | 121.22 (12) |
C15—Mn—C14 | 37.96 (12) | C33—C28—P1 | 118.79 (12) |
C13—Mn—C14 | 38.14 (12) | C30—C29—C28 | 120.0 |
C4—Mn—Pt | 106.38 (11) | C30—C29—H29 | 120.0 |
C3—Mn—Pt | 62.03 (9) | C28—C29—H29 | 120.0 |
C1—Mn—Pt | 49.08 (8) | C31—C30—C29 | 120.0 |
C12—Mn—Pt | 149.66 (10) | C31—C30—H30 | 120.0 |
C11—Mn—Pt | 148.89 (11) | C29—C30—H30 | 120.0 |
C15—Mn—Pt | 111.32 (10) | C30—C31—C32 | 120.0 |
C13—Mn—Pt | 111.97 (9) | C30—C31—H31 | 120.0 |
C14—Mn—Pt | 93.71 (9) | C32—C31—H31 | 120.0 |
O3—C3—Mn | 166.0 (3) | C33—C32—C31 | 120.0 |
O3—C3—Pt | 117.7 (2) | C33—C32—H32 | 120.0 |
Mn—C3—Pt | 76.11 (11) | C31—C32—H32 | 120.0 |
O4—C4—Mn | 178.9 (4) | C32—C33—C28 | 120.0 |
C15—C11—C12 | 107.3 (3) | C32—C33—H33 | 120.0 |
C15—C11—Mn | 71.82 (19) | C28—C33—H33 | 120.0 |
C12—C11—Mn | 70.36 (18) | C40—P2—C46 | 105.87 (11) |
C15—C11—H11 | 126.3 | C40—P2—C34 | 99.64 (10) |
C12—C11—H11 | 126.3 | C46—P2—C34 | 103.53 (11) |
Mn—C11—H11 | 123.2 | C40—P2—Pt | 123.19 (7) |
C13—C12—C11 | 108.1 (3) | C46—P2—Pt | 108.16 (8) |
C13—C12—Mn | 72.27 (18) | C34—P2—Pt | 114.51 (8) |
C11—C12—Mn | 70.51 (18) | C35—C34—C39 | 120.0 |
C13—C12—H12 | 125.9 | C35—C34—P2 | 118.32 (14) |
C11—C12—H12 | 125.9 | C39—C34—P2 | 121.55 (14) |
Mn—C12—H12 | 122.9 | C36—C35—C34 | 120.0 |
C12—C13—C14 | 108.1 (3) | C36—C35—H35 | 120.0 |
C12—C13—Mn | 69.84 (18) | C34—C35—H35 | 120.0 |
C14—C13—Mn | 71.28 (18) | C35—C36—C37 | 120.0 |
C12—C13—H13 | 126.0 | C35—C36—H36 | 120.0 |
C14—C13—H13 | 126.0 | C37—C36—H36 | 120.0 |
Mn—C13—H13 | 124.5 | C38—C37—C36 | 120.0 |
C15—C14—C13 | 107.5 (3) | C38—C37—H37 | 120.0 |
C15—C14—Mn | 70.31 (19) | C36—C37—H37 | 120.0 |
C13—C14—Mn | 70.58 (17) | C39—C38—C37 | 120.0 |
C15—C14—H14 | 126.2 | C39—C38—H38 | 120.0 |
C13—C14—H14 | 126.2 | C37—C38—H38 | 120.0 |
Mn—C14—H14 | 124.5 | C38—C39—C34 | 120.0 |
C11—C15—C14 | 108.9 (3) | C38—C39—H39 | 120.0 |
C11—C15—Mn | 70.27 (19) | C34—C39—H39 | 120.0 |
C14—C15—Mn | 71.73 (18) | C41—C40—C45 | 120.0 |
C11—C15—H15 | 125.5 | C41—C40—P2 | 121.08 (12) |
C14—C15—H15 | 125.5 | C45—C40—P2 | 118.90 (12) |
Mn—C15—H15 | 124.1 | C42—C41—C40 | 120.0 |
C2—C1—Mn | 141.0 (2) | C42—C41—H41 | 120.0 |
C2—C1—Pt | 135.2 (2) | C40—C41—H41 | 120.0 |
Mn—C1—Pt | 82.93 (11) | C41—C42—C43 | 120.0 |
C1—C2—C5 | 131.9 (3) | C41—C42—H42 | 120.0 |
C1—C2—H2 | 114.1 | C43—C42—H42 | 120.0 |
C5—C2—H2 | 114.1 | C44—C43—C42 | 120.0 |
C6—C5—C10 | 120.0 | C44—C43—H43 | 120.0 |
C6—C5—C2 | 117.66 (18) | C42—C43—H43 | 120.0 |
C10—C5—C2 | 122.32 (18) | C43—C44—C45 | 120.0 |
C5—C6—C7 | 120.0 | C43—C44—H44 | 120.0 |
C5—C6—H6 | 120.0 | C45—C44—H44 | 120.0 |
C7—C6—H6 | 120.0 | C44—C45—C40 | 120.0 |
C8—C7—C6 | 120.0 | C44—C45—H45 | 120.0 |
C8—C7—H7 | 120.0 | C40—C45—H45 | 120.0 |
C6—C7—H7 | 120.0 | C47—C46—C51 | 120.0 |
C9—C8—C7 | 120.0 | C47—C46—P2 | 116.51 (15) |
C9—C8—H8 | 120.0 | C51—C46—P2 | 123.45 (15) |
C7—C8—H8 | 120.0 | C48—C47—C46 | 120.0 |
C8—C9—C10 | 120.0 | C48—C47—H47 | 120.0 |
C8—C9—H9 | 120.0 | C46—C47—H47 | 120.0 |
C10—C9—H9 | 120.0 | C47—C48—C49 | 120.0 |
C9—C10—C5 | 120.0 | C47—C48—H48 | 120.0 |
C9—C10—H10 | 120.0 | C49—C48—H48 | 120.0 |
C5—C10—H10 | 120.0 | C50—C49—C48 | 120.0 |
C22—P1—C28 | 100.62 (9) | C50—C49—H49 | 120.0 |
C22—P1—C16 | 102.59 (9) | C48—C49—H49 | 120.0 |
C28—P1—C16 | 103.64 (10) | C49—C50—C51 | 120.0 |
C22—P1—Pt | 120.73 (7) | C49—C50—H50 | 120.0 |
C28—P1—Pt | 115.63 (7) | C51—C50—H50 | 120.0 |
C16—P1—Pt | 111.49 (6) | C50—C51—C46 | 120.0 |
C17—C16—C21 | 120.0 | C50—C51—H51 | 120.0 |
C17—C16—P1 | 120.84 (11) | C46—C51—H51 | 120.0 |
Experimental details
Crystal data | |
Chemical formula | [MnPt(C5H5)(C8H6)(C18H15P)2(CO)2] |
Mr | 997.81 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 283 |
a, b, c (Å) | 11.1320 (4), 19.4463 (7), 19.5174 (7) |
V (Å3) | 4225.1 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.72 |
Crystal size (mm) | 0.29 × 0.17 × 0.14 |
Data collection | |
Diffractometer | Bruker SMART 4K CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2004) |
Tmin, Tmax | 0.352, 0.624 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 37385, 9675, 8974 |
Rint | 0.026 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.020, 0.045, 0.95 |
No. of reflections | 9675 |
No. of parameters | 433 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.63, −0.25 |
Absolute structure | Flack (1983), 4291 Friedel pairs |
Absolute structure parameter | −0.007 (3) |
Computer programs: SMART (Bruker, 1998), SMART, SAINT (Bruker, 1998), SHELXTL (Sheldrick, 1997), SHELXTL.
Pt—C1 | 2.006 (3) | Mn—C4 | 1.761 (4) |
Pt—C3 | 2.397 (3) | Mn—C11 | 2.129 (3) |
Pt—P1 | 2.2745 (7) | Mn—C12 | 2.127 (3) |
Pt—P2 | 2.3548 (8) | Mn—C13 | 2.158 (3) |
Pt—Mn | 2.6344 (4) | Mn—C14 | 2.167 (3) |
Mn—C1 | 1.972 (3) | Mn—C15 | 2.149 (3) |
Mn—C3 | 1.811 (3) |
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The molecule of the title compound, (I), is the dinuclear complex containing the Mn and Pt atoms bridged by the µ-phenylvinylidene ligand and semi-bridged by carbonyl group. The phenyl ring and the C?C bond of vinylidene coupling with the Mn—Pt-µ-C triangle form an almost planar system. Corresponding geometry was found for the related MnPt complex with chelating bis(diphenylphosphino)methane at the Pt atom (Dolgushin et al., 2001). The structures of some µ-carbene complexes containing the Mn—Pt-µ-C triangle system as a molecular central fragment were reported (Jeffery et al., 1981).