Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801017500/bt6085sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801017500/bt6085Isup2.hkl |
CCDC reference: 175985
Key indicators
- Single-crystal X-ray study
- T = 110 K
- Mean (C-C) = 0.010 Å
- Disorder in solvent or counterion
- R factor = 0.054
- wR factor = 0.129
- Data-to-parameter ratio = 21.0
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 5 PLAT_302 Alert C Anion/Solvent Disorder ....................... 50.00 Perc. PLAT_320 Alert C Check Hybridisation of C1 in main residue ? PLAT_320 Alert C Check Hybridisation of C3 in main residue ? General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.651 Tmax scaled 0.452 Tmin scaled 0.289
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
4 Alert Level C = Please check
The title compound was prepared according to a known procedure (Antonova et al., 1991). Suitable single crystals were obtained by isothermic evaporation of a solution in benzene–ether (2:1) at 258 K.
The solvate diethyl ether molecule is disordered over two positions with occupancies of 0.6 and 0.4. A l l atoms of the solvate molecules were refined isotropically and the C—O and C—C distances were restrained by the DFIX instruction to values of 1.426 and 1.530 Å, respectively (Allen et al., 1987). H atoms were placed in calculated positions with Uiso constrained to be 1.2 times Ueq of the carrier atom. The highest peak in the final difference map is 0.91 Å from the Mn atom.
Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[MnPt(C5H5)(C8H6)(C25H22P2)(CO)2]·C4H10O | Dx = 1.565 Mg m−3 |
Mr = 931.75 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pbca | Cell parameters from 932 reflections |
a = 18.3417 (18) Å | θ = 2–24° |
b = 18.3164 (18) Å | µ = 3.97 mm−1 |
c = 23.547 (2) Å | T = 110 K |
V = 7910.7 (14) Å3 | Prism, orange |
Z = 8 | 0.4 × 0.2 × 0.2 mm |
F(000) = 3712 |
CCD area detector diffractometer | 9557 independent reflections |
Radiation source: fine-focus sealed tube | 5404 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.070 |
ϕ and ω scans | θmax = 28.1°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1998) | h = −24→23 |
Tmin = 0.443, Tmax = 0.694 | k = −24→11 |
55551 measured reflections | l = −31→31 |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.129 | H-atom parameters constrained |
S = 0.97 | w = 1/[σ2(Fo2) + (0.06P)2] where P = (Fo2 + 2Fc2)/3 |
9557 reflections | (Δ/σ)max = 0.001 |
455 parameters | Δρmax = 1.91 e Å−3 |
8 restraints | Δρmin = −1.67 e Å−3 |
[MnPt(C5H5)(C8H6)(C25H22P2)(CO)2]·C4H10O | V = 7910.7 (14) Å3 |
Mr = 931.75 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 18.3417 (18) Å | µ = 3.97 mm−1 |
b = 18.3164 (18) Å | T = 110 K |
c = 23.547 (2) Å | 0.4 × 0.2 × 0.2 mm |
CCD area detector diffractometer | 9557 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1998) | 5404 reflections with I > 2σ(I) |
Tmin = 0.443, Tmax = 0.694 | Rint = 0.070 |
55551 measured reflections |
R[F2 > 2σ(F2)] = 0.054 | 8 restraints |
wR(F2) = 0.129 | H-atom parameters constrained |
S = 0.97 | Δρmax = 1.91 e Å−3 |
9557 reflections | Δρmin = −1.67 e Å−3 |
455 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 | Occ. (<1) | |
Pt1 | 0.044444 (12) | 0.367216 (14) | −0.326505 (10) | 0.02265 (9) | |
Mn1 | −0.01953 (5) | 0.38471 (6) | −0.42442 (4) | 0.0274 (2) | |
P1 | 0.16410 (9) | 0.37428 (10) | −0.29358 (7) | 0.0242 (4) | |
P2 | 0.04716 (9) | 0.31278 (9) | −0.23948 (7) | 0.0233 (4) | |
O3 | 0.1075 (2) | 0.4804 (3) | −0.4095 (2) | 0.0408 (13) | |
O4 | −0.1138 (3) | 0.5129 (3) | −0.4137 (2) | 0.0384 (12) | |
C1 | −0.0544 (3) | 0.3415 (4) | −0.3551 (3) | 0.0261 (15) | |
C2 | −0.1100 (3) | 0.3015 (3) | −0.3324 (3) | 0.0248 (14) | |
H2A | −0.1034 | 0.2841 | −0.2948 | 0.030* | |
C3 | 0.0602 (4) | 0.4371 (4) | −0.4022 (3) | 0.0329 (17) | |
C4 | −0.0762 (4) | 0.4626 (4) | −0.4161 (3) | 0.0308 (16) | |
C5 | −0.1790 (3) | 0.2829 (4) | −0.3605 (3) | 0.0253 (15) | |
C6 | −0.2163 (3) | 0.3290 (4) | −0.3968 (3) | 0.0307 (16) | |
H6A | −0.1977 | 0.3768 | −0.4029 | 0.037* | |
C7 | −0.2799 (4) | 0.3084 (4) | −0.4246 (3) | 0.0382 (18) | |
H7A | −0.3030 | 0.3413 | −0.4501 | 0.046* | |
C8 | −0.3098 (4) | 0.2393 (4) | −0.4153 (3) | 0.0373 (19) | |
H8A | −0.3536 | 0.2248 | −0.4337 | 0.045* | |
C9 | −0.2739 (4) | 0.1923 (4) | −0.3784 (3) | 0.0355 (17) | |
H9A | −0.2933 | 0.1449 | −0.3719 | 0.043* | |
C10 | −0.2107 (3) | 0.2130 (4) | −0.3508 (3) | 0.0308 (16) | |
H10A | −0.1881 | 0.1802 | −0.3250 | 0.037* | |
C11 | −0.0239 (4) | 0.3875 (4) | −0.5146 (3) | 0.0408 (19) | |
H11A | −0.0310 | 0.4325 | −0.5380 | 0.049* | |
C12 | −0.0801 (4) | 0.3434 (5) | −0.4936 (3) | 0.047 (2) | |
H12A | −0.1336 | 0.3500 | −0.5003 | 0.057* | |
C13 | −0.0467 (4) | 0.2844 (4) | −0.4656 (3) | 0.0407 (19) | |
H13A | −0.0729 | 0.2425 | −0.4475 | 0.049* | |
C14 | 0.0297 (4) | 0.2925 (4) | −0.4686 (3) | 0.042 (2) | |
H14A | 0.0673 | 0.2582 | −0.4533 | 0.050* | |
C15 | 0.0425 (4) | 0.3591 (4) | −0.4991 (3) | 0.0365 (17) | |
H15A | 0.0913 | 0.3797 | −0.5092 | 0.044* | |
C16 | 0.1459 (3) | 0.3207 (4) | −0.2284 (3) | 0.0302 (16) | |
H16A | 0.1708 | 0.2727 | −0.2286 | 0.036* | |
H16B | 0.1583 | 0.3478 | −0.1933 | 0.036* | |
C17 | 0.2152 (3) | 0.4545 (4) | −0.2706 (3) | 0.0267 (15) | |
C18 | 0.2718 (4) | 0.4482 (4) | −0.2319 (3) | 0.0342 (17) | |
H18A | 0.2810 | 0.4025 | −0.2142 | 0.041* | |
C19 | 0.3151 (4) | 0.5077 (4) | −0.2188 (3) | 0.0384 (18) | |
H19A | 0.3544 | 0.5027 | −0.1928 | 0.046* | |
C20 | 0.3005 (4) | 0.5750 (4) | −0.2441 (3) | 0.043 (2) | |
H20A | 0.3302 | 0.6161 | −0.2358 | 0.052* | |
C21 | 0.2445 (4) | 0.5814 (4) | −0.2801 (4) | 0.045 (2) | |
H21A | 0.2339 | 0.6278 | −0.2962 | 0.054* | |
C22 | 0.2008 (4) | 0.5213 (4) | −0.2948 (3) | 0.0401 (19) | |
H22A | 0.1620 | 0.5267 | −0.3211 | 0.048* | |
C23 | 0.2321 (3) | 0.3227 (3) | −0.3333 (3) | 0.0256 (15) | |
C24 | 0.2859 (3) | 0.2822 (4) | −0.3060 (3) | 0.0324 (17) | |
H24A | 0.2862 | 0.2785 | −0.2658 | 0.039* | |
C25 | 0.3386 (4) | 0.2477 (4) | −0.3377 (3) | 0.0365 (18) | |
H25A | 0.3745 | 0.2191 | −0.3190 | 0.044* | |
C26 | 0.3404 (4) | 0.2536 (4) | −0.3953 (4) | 0.044 (2) | |
H26A | 0.3777 | 0.2300 | −0.4164 | 0.053* | |
C27 | 0.2872 (4) | 0.2945 (5) | −0.4230 (3) | 0.049 (2) | |
H27A | 0.2881 | 0.2984 | −0.4632 | 0.058* | |
C28 | 0.2331 (4) | 0.3293 (4) | −0.3923 (3) | 0.0370 (18) | |
H28A | 0.1970 | 0.3574 | −0.4112 | 0.044* | |
C29 | 0.0043 (3) | 0.3587 (3) | −0.1806 (3) | 0.0270 (15) | |
C30 | −0.0548 (3) | 0.3999 (3) | −0.1862 (3) | 0.0342 (14) | |
H30A | −0.0725 | 0.4031 | −0.2241 | 0.041* | |
C31 | −0.0941 (4) | 0.4375 (4) | −0.1487 (4) | 0.045 (2) | |
H31A | −0.1369 | 0.4638 | −0.1586 | 0.054* | |
C32 | −0.0670 (4) | 0.4349 (5) | −0.0937 (3) | 0.048 (2) | |
H32A | −0.0911 | 0.4604 | −0.0640 | 0.057* | |
C33 | −0.0026 (5) | 0.3936 (5) | −0.0821 (3) | 0.047 (2) | |
H33A | 0.0167 | 0.3914 | −0.0446 | 0.056* | |
C34 | 0.0311 (4) | 0.3571 (5) | −0.1259 (3) | 0.047 (2) | |
H34A | 0.0741 | 0.3299 | −0.1183 | 0.056* | |
C35 | 0.0256 (3) | 0.2158 (4) | −0.2325 (3) | 0.0289 (16) | |
C36 | 0.0183 (4) | 0.1813 (4) | −0.1802 (3) | 0.0321 (16) | |
H36A | 0.0238 | 0.2082 | −0.1460 | 0.039* | |
C37 | 0.0028 (4) | 0.1072 (4) | −0.1783 (4) | 0.046 (2) | |
H37A | −0.0017 | 0.0835 | −0.1426 | 0.055* | |
C38 | −0.0061 (4) | 0.0676 (4) | −0.2273 (4) | 0.043 (2) | |
H38A | −0.0169 | 0.0170 | −0.2252 | 0.052* | |
C39 | 0.0006 (4) | 0.1006 (4) | −0.2791 (4) | 0.048 (2) | |
H39A | −0.0055 | 0.0731 | −0.3129 | 0.057* | |
C40 | 0.0165 (4) | 0.1757 (4) | −0.2819 (3) | 0.0322 (16) | |
H40A | 0.0210 | 0.1990 | −0.3178 | 0.039* | |
O1S | −0.3286 (6) | 0.4488 (6) | −0.5138 (5) | 0.059 (3)* | 0.60 |
C1S | −0.2886 (14) | 0.4251 (18) | −0.5619 (12) | 0.096 (12)* | 0.60 |
H1SA | −0.2425 | 0.4009 | −0.5509 | 0.115* | 0.60 |
H1SB | −0.2779 | 0.4660 | −0.5881 | 0.115* | 0.60 |
C2S | −0.3444 (10) | 0.3697 (9) | −0.5883 (7) | 0.078 (5)* | 0.60 |
H2SA | −0.3224 | 0.3460 | −0.6215 | 0.117* | 0.60 |
H2SB | −0.3886 | 0.3958 | −0.6000 | 0.117* | 0.60 |
H2SC | −0.3570 | 0.3325 | −0.5600 | 0.117* | 0.60 |
C3S | −0.2884 (10) | 0.5037 (10) | −0.4830 (8) | 0.079 (5)* | 0.60 |
H3SA | −0.2809 | 0.5471 | −0.5074 | 0.095* | 0.60 |
H3SB | −0.2400 | 0.4844 | −0.4721 | 0.095* | 0.60 |
C4S | −0.3317 (16) | 0.5252 (18) | −0.4294 (11) | 0.145 (12)* | 0.60 |
H4SA | −0.3038 | 0.5610 | −0.4074 | 0.218* | 0.60 |
H4SB | −0.3404 | 0.4817 | −0.4061 | 0.218* | 0.60 |
H4SC | −0.3785 | 0.5466 | −0.4406 | 0.218* | 0.60 |
O1S' | −0.3303 (8) | 0.4741 (9) | −0.4902 (7) | 0.060 (5)* | 0.40 |
C1S' | −0.2659 (12) | 0.4717 (14) | −0.5268 (10) | 0.074 (7)* | 0.40 |
H1SC | −0.2213 | 0.4571 | −0.5060 | 0.089* | 0.40 |
H1SD | −0.2575 | 0.5183 | −0.5471 | 0.089* | 0.40 |
C2S' | −0.295 (2) | 0.411 (2) | −0.5662 (17) | 0.083 (16)* | 0.40 |
H2SD | −0.2584 | 0.3998 | −0.5954 | 0.124* | 0.40 |
H2SE | −0.3401 | 0.4270 | −0.5844 | 0.124* | 0.40 |
H2SF | −0.3045 | 0.3666 | −0.5438 | 0.124* | 0.40 |
C3S' | −0.3145 (13) | 0.5298 (13) | −0.4506 (11) | 0.054 (6)* | 0.40 |
H3SC | −0.3067 | 0.5764 | −0.4710 | 0.065* | 0.40 |
H3SD | −0.2690 | 0.5177 | −0.4301 | 0.065* | 0.40 |
C4S' | −0.3766 (18) | 0.539 (2) | −0.4082 (14) | 0.139 (15)* | 0.40 |
H4SD | −0.3644 | 0.5774 | −0.3811 | 0.208* | 0.40 |
H4SE | −0.3839 | 0.4927 | −0.3877 | 0.208* | 0.40 |
H4SF | −0.4214 | 0.5516 | −0.4285 | 0.208* | 0.40 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.01812 (13) | 0.02450 (14) | 0.02534 (14) | 0.00018 (11) | −0.00125 (10) | 0.00279 (12) |
Mn1 | 0.0235 (5) | 0.0341 (6) | 0.0246 (5) | 0.0009 (4) | −0.0011 (4) | 0.0022 (5) |
P1 | 0.0174 (8) | 0.0285 (10) | 0.0266 (9) | 0.0010 (7) | 0.0012 (7) | 0.0018 (8) |
P2 | 0.0188 (8) | 0.0232 (9) | 0.0278 (9) | 0.0009 (7) | −0.0006 (7) | 0.0021 (7) |
O3 | 0.030 (3) | 0.043 (3) | 0.050 (3) | −0.008 (2) | −0.005 (2) | 0.018 (3) |
O4 | 0.034 (3) | 0.033 (3) | 0.049 (3) | 0.006 (2) | −0.003 (2) | 0.002 (3) |
C1 | 0.025 (4) | 0.026 (3) | 0.027 (4) | −0.001 (3) | 0.000 (3) | 0.001 (3) |
C2 | 0.027 (3) | 0.022 (3) | 0.026 (3) | 0.001 (3) | 0.000 (3) | 0.001 (3) |
C3 | 0.040 (4) | 0.027 (4) | 0.032 (4) | 0.006 (3) | 0.000 (3) | 0.005 (3) |
C4 | 0.024 (4) | 0.040 (4) | 0.028 (4) | −0.007 (3) | −0.004 (3) | 0.004 (3) |
C5 | 0.025 (4) | 0.028 (4) | 0.023 (3) | −0.002 (3) | 0.005 (3) | −0.003 (3) |
C6 | 0.026 (4) | 0.032 (4) | 0.034 (4) | −0.003 (3) | 0.002 (3) | 0.003 (3) |
C7 | 0.029 (4) | 0.050 (5) | 0.036 (4) | 0.004 (4) | −0.002 (3) | 0.012 (4) |
C8 | 0.023 (4) | 0.048 (5) | 0.041 (4) | −0.007 (3) | −0.006 (3) | −0.013 (4) |
C9 | 0.035 (4) | 0.031 (4) | 0.040 (4) | −0.004 (3) | 0.008 (3) | −0.007 (4) |
C10 | 0.024 (4) | 0.033 (4) | 0.036 (4) | 0.000 (3) | 0.002 (3) | −0.001 (3) |
C11 | 0.061 (5) | 0.043 (5) | 0.018 (3) | 0.013 (4) | 0.004 (3) | 0.002 (3) |
C12 | 0.039 (5) | 0.070 (6) | 0.032 (4) | −0.002 (4) | −0.003 (4) | −0.021 (4) |
C13 | 0.056 (5) | 0.035 (4) | 0.031 (4) | −0.011 (4) | 0.007 (4) | −0.011 (3) |
C14 | 0.054 (5) | 0.038 (4) | 0.033 (4) | 0.013 (4) | 0.002 (4) | −0.001 (4) |
C15 | 0.033 (4) | 0.045 (5) | 0.032 (4) | 0.002 (4) | 0.011 (3) | −0.003 (4) |
C16 | 0.020 (3) | 0.032 (4) | 0.039 (4) | 0.004 (3) | −0.003 (3) | 0.007 (3) |
C17 | 0.021 (3) | 0.025 (4) | 0.035 (4) | 0.002 (3) | 0.002 (3) | −0.004 (3) |
C18 | 0.032 (4) | 0.032 (4) | 0.039 (4) | −0.001 (3) | −0.005 (3) | 0.007 (3) |
C19 | 0.036 (4) | 0.038 (4) | 0.041 (4) | −0.010 (4) | −0.011 (3) | 0.003 (4) |
C20 | 0.039 (5) | 0.032 (4) | 0.058 (5) | 0.001 (4) | 0.010 (4) | −0.006 (4) |
C21 | 0.048 (5) | 0.028 (4) | 0.058 (5) | 0.002 (4) | −0.010 (4) | 0.006 (4) |
C22 | 0.032 (4) | 0.036 (4) | 0.053 (5) | 0.001 (3) | −0.008 (4) | 0.001 (4) |
C23 | 0.023 (3) | 0.011 (3) | 0.043 (4) | 0.003 (2) | 0.003 (3) | −0.008 (3) |
C24 | 0.023 (4) | 0.033 (4) | 0.041 (4) | −0.002 (3) | −0.004 (3) | −0.009 (3) |
C25 | 0.021 (4) | 0.033 (4) | 0.055 (5) | 0.001 (3) | 0.001 (3) | −0.009 (4) |
C26 | 0.036 (4) | 0.041 (5) | 0.056 (5) | 0.000 (4) | 0.005 (4) | −0.015 (4) |
C27 | 0.051 (5) | 0.058 (6) | 0.037 (5) | −0.001 (4) | 0.009 (4) | −0.011 (4) |
C28 | 0.037 (4) | 0.038 (4) | 0.036 (4) | 0.001 (3) | 0.004 (4) | −0.001 (4) |
C29 | 0.017 (3) | 0.025 (4) | 0.039 (4) | 0.000 (3) | 0.001 (3) | 0.001 (3) |
C30 | 0.027 (3) | 0.032 (3) | 0.042 (4) | 0.003 (2) | 0.016 (3) | 0.003 (3) |
C31 | 0.027 (4) | 0.039 (5) | 0.069 (6) | 0.011 (3) | 0.004 (4) | 0.008 (4) |
C32 | 0.056 (5) | 0.052 (5) | 0.035 (4) | 0.017 (4) | 0.012 (4) | −0.005 (4) |
C33 | 0.065 (6) | 0.055 (5) | 0.021 (4) | −0.004 (4) | 0.009 (4) | −0.012 (4) |
C34 | 0.048 (5) | 0.053 (6) | 0.040 (5) | 0.016 (4) | 0.001 (4) | 0.006 (4) |
C35 | 0.023 (3) | 0.021 (3) | 0.043 (4) | 0.001 (3) | −0.001 (3) | 0.003 (3) |
C36 | 0.026 (3) | 0.033 (4) | 0.037 (4) | 0.009 (3) | 0.003 (3) | 0.008 (3) |
C37 | 0.026 (4) | 0.034 (4) | 0.077 (6) | 0.002 (3) | 0.012 (4) | 0.026 (5) |
C38 | 0.038 (4) | 0.016 (4) | 0.076 (6) | 0.002 (3) | 0.000 (4) | 0.003 (4) |
C39 | 0.047 (5) | 0.025 (4) | 0.072 (6) | −0.004 (4) | −0.011 (4) | 0.003 (4) |
C40 | 0.032 (4) | 0.029 (4) | 0.035 (4) | 0.002 (3) | −0.008 (3) | −0.001 (3) |
Pt1—Mn1 | 2.6068 (10) | C14—C15 | 1.435 (10) |
Pt1—P1 | 2.3312 (16) | C17—C22 | 1.374 (9) |
Pt1—P2 | 2.2796 (17) | C17—C18 | 1.386 (9) |
Pt1—C1 | 1.991 (6) | C18—C19 | 1.382 (9) |
Pt1—C3 | 2.212 (7) | C19—C20 | 1.395 (10) |
Mn1—C1 | 1.924 (7) | C20—C21 | 1.337 (10) |
Mn1—C3 | 1.826 (7) | C21—C22 | 1.404 (10) |
Mn1—C4 | 1.775 (8) | C23—C24 | 1.392 (9) |
Mn1—C11 | 2.126 (7) | C23—C28 | 1.395 (9) |
Mn1—C12 | 2.112 (7) | C24—C25 | 1.376 (9) |
Mn1—C13 | 2.137 (7) | C25—C26 | 1.359 (10) |
Mn1—C14 | 2.178 (7) | C26—C27 | 1.391 (11) |
Mn1—C15 | 2.146 (7) | C27—C28 | 1.384 (10) |
P2—C29 | 1.801 (7) | C29—C30 | 1.329 (8) |
P2—C35 | 1.827 (7) | C29—C34 | 1.379 (10) |
P2—C16 | 1.835 (6) | C30—C31 | 1.333 (9) |
P1—C23 | 1.822 (6) | C31—C32 | 1.386 (11) |
P1—C17 | 1.825 (7) | C32—C33 | 1.429 (11) |
P1—C16 | 1.852 (7) | C33—C34 | 1.378 (10) |
O3—C3 | 1.189 (8) | C35—C40 | 1.386 (9) |
O4—C4 | 1.153 (8) | C35—C36 | 1.391 (9) |
C1—C2 | 1.363 (9) | C36—C37 | 1.386 (11) |
C2—C5 | 1.469 (9) | C37—C38 | 1.372 (11) |
C5—C6 | 1.383 (9) | C38—C39 | 1.366 (11) |
C5—C10 | 1.424 (9) | C39—C40 | 1.408 (10) |
C6—C7 | 1.390 (9) | O1S—C1S | 1.418 (18) |
C7—C8 | 1.397 (10) | O1S—C3S | 1.442 (14) |
C8—C9 | 1.388 (10) | C1S—C2S | 1.570 (17) |
C9—C10 | 1.382 (9) | C3S—C4S | 1.543 (17) |
C11—C15 | 1.373 (10) | O1S'—C3S' | 1.412 (17) |
C11—C12 | 1.401 (11) | O1S'—C1S' | 1.464 (17) |
C12—C13 | 1.407 (11) | C1S'—C2S' | 1.548 (19) |
C13—C14 | 1.410 (10) | C3S'—C4S' | 1.524 (19) |
C1—Pt1—C3 | 89.1 (3) | Mn1—C3—Pt1 | 79.8 (3) |
C1—Pt1—P2 | 102.7 (2) | O4—C4—Mn1 | 176.3 (6) |
C3—Pt1—P2 | 166.9 (2) | C6—C5—C10 | 116.6 (6) |
C1—Pt1—P1 | 169.4 (2) | C6—C5—C2 | 124.2 (6) |
C3—Pt1—P1 | 96.47 (19) | C10—C5—C2 | 119.3 (6) |
P2—Pt1—P1 | 72.83 (6) | C5—C6—C7 | 122.6 (7) |
C1—Pt1—Mn1 | 47.17 (19) | C6—C7—C8 | 120.1 (7) |
C3—Pt1—Mn1 | 43.57 (19) | C9—C8—C7 | 118.2 (6) |
P2—Pt1—Mn1 | 149.17 (5) | C10—C9—C8 | 121.5 (7) |
P1—Pt1—Mn1 | 135.32 (5) | C9—C10—C5 | 120.9 (7) |
C4—Mn1—C3 | 90.8 (3) | C15—C11—C12 | 109.9 (7) |
C4—Mn1—C1 | 92.4 (3) | C15—C11—Mn1 | 72.0 (4) |
C3—Mn1—C1 | 103.8 (3) | C12—C11—Mn1 | 70.1 (4) |
C4—Mn1—C12 | 93.7 (3) | C11—C12—C13 | 106.7 (7) |
C3—Mn1—C12 | 146.2 (3) | C11—C12—Mn1 | 71.3 (4) |
C1—Mn1—C12 | 109.4 (3) | C13—C12—Mn1 | 71.6 (4) |
C4—Mn1—C11 | 94.0 (3) | C12—C13—C14 | 109.1 (7) |
C3—Mn1—C11 | 107.7 (3) | C12—C13—Mn1 | 69.7 (4) |
C1—Mn1—C11 | 147.7 (3) | C14—C13—Mn1 | 72.5 (4) |
C12—Mn1—C11 | 38.6 (3) | C13—C14—C15 | 106.1 (7) |
C4—Mn1—C13 | 127.2 (3) | C13—C14—Mn1 | 69.3 (4) |
C3—Mn1—C13 | 140.3 (3) | C15—C14—Mn1 | 69.4 (4) |
C1—Mn1—C13 | 87.3 (3) | C11—C15—C14 | 108.0 (7) |
C12—Mn1—C13 | 38.7 (3) | C11—C15—Mn1 | 70.5 (4) |
C11—Mn1—C13 | 63.8 (3) | C14—C15—Mn1 | 71.8 (4) |
C4—Mn1—C15 | 125.2 (3) | P2—C16—P1 | 95.9 (3) |
C3—Mn1—C15 | 85.7 (3) | C22—C17—C18 | 119.3 (6) |
C1—Mn1—C15 | 141.4 (3) | C22—C17—P1 | 119.7 (5) |
C12—Mn1—C15 | 64.5 (3) | C18—C17—P1 | 120.8 (5) |
C11—Mn1—C15 | 37.5 (3) | C19—C18—C17 | 120.8 (7) |
C13—Mn1—C15 | 64.2 (3) | C18—C19—C20 | 119.4 (7) |
C4—Mn1—C14 | 156.6 (3) | C21—C20—C19 | 119.7 (7) |
C3—Mn1—C14 | 102.3 (3) | C20—C21—C22 | 121.7 (7) |
C1—Mn1—C14 | 102.9 (3) | C17—C22—C21 | 119.1 (7) |
C12—Mn1—C14 | 64.7 (3) | C24—C23—C28 | 119.8 (6) |
C11—Mn1—C14 | 63.7 (3) | C24—C23—P1 | 121.6 (5) |
C13—Mn1—C14 | 38.1 (3) | C28—C23—P1 | 118.4 (5) |
C15—Mn1—C14 | 38.8 (3) | C25—C24—C23 | 119.5 (7) |
C4—Mn1—Pt1 | 105.3 (2) | C26—C25—C24 | 121.4 (7) |
C3—Mn1—Pt1 | 56.6 (2) | C25—C26—C27 | 119.6 (7) |
C1—Mn1—Pt1 | 49.35 (19) | C28—C27—C26 | 120.3 (8) |
C12—Mn1—Pt1 | 151.0 (3) | C27—C28—C23 | 119.4 (7) |
C11—Mn1—Pt1 | 154.6 (2) | C30—C29—C34 | 113.3 (6) |
C13—Mn1—Pt1 | 113.6 (2) | C30—C29—P2 | 123.1 (5) |
C15—Mn1—Pt1 | 117.3 (2) | C34—C29—P2 | 123.6 (5) |
C14—Mn1—Pt1 | 98.1 (2) | C29—C30—C31 | 132.0 (7) |
C29—P2—C35 | 106.9 (3) | C30—C31—C32 | 114.0 (7) |
C29—P2—C16 | 106.5 (3) | C31—C32—C33 | 119.6 (7) |
C35—P2—C16 | 106.1 (3) | C34—C33—C32 | 118.9 (7) |
C29—P2—Pt1 | 118.6 (2) | C33—C34—C29 | 122.0 (7) |
C35—P2—Pt1 | 120.1 (2) | C40—C35—C36 | 119.4 (6) |
C16—P2—Pt1 | 96.6 (2) | C40—C35—P2 | 117.8 (5) |
C23—P1—C17 | 102.6 (3) | C36—C35—P2 | 122.9 (5) |
C23—P1—C16 | 105.9 (3) | C37—C36—C35 | 119.6 (7) |
C17—P1—C16 | 105.9 (3) | C38—C37—C36 | 121.0 (7) |
C23—P1—Pt1 | 116.4 (2) | C39—C38—C37 | 120.4 (7) |
C17—P1—Pt1 | 128.8 (2) | C38—C39—C40 | 119.6 (8) |
C16—P1—Pt1 | 94.4 (2) | C35—C40—C39 | 120.2 (7) |
C2—C1—Mn1 | 143.2 (5) | C1S—O1S—C3S | 110.5 (13) |
C2—C1—Pt1 | 132.5 (5) | O1S—C1S—C2S | 100.3 (15) |
Mn1—C1—Pt1 | 83.5 (2) | O1S—C3S—C4S | 109.0 (17) |
C1—C2—C5 | 126.5 (6) | C3S'—O1S'—C1S' | 104.1 (17) |
O3—C3—Mn1 | 153.4 (6) | O1S'—C1S'—C2S' | 96 (2) |
O3—C3—Pt1 | 126.7 (5) | O1S'—C3S'—C4S' | 111 (2) |
Experimental details
Crystal data | |
Chemical formula | [MnPt(C5H5)(C8H6)(C25H22P2)(CO)2]·C4H10O |
Mr | 931.75 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 110 |
a, b, c (Å) | 18.3417 (18), 18.3164 (18), 23.547 (2) |
V (Å3) | 7910.7 (14) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 3.97 |
Crystal size (mm) | 0.4 × 0.2 × 0.2 |
Data collection | |
Diffractometer | CCD area detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1998) |
Tmin, Tmax | 0.443, 0.694 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 55551, 9557, 5404 |
Rint | 0.070 |
(sin θ/λ)max (Å−1) | 0.663 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.054, 0.129, 0.97 |
No. of reflections | 9557 |
No. of parameters | 455 |
No. of restraints | 8 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.91, −1.67 |
Computer programs: SMART (Bruker, 1998), SAINT-Plus (Bruker, 1998), SAINT-Plus, SHELXTL (Sheldrick, 1998), SHELXTL.
Pt1—Mn1 | 2.6068 (10) | Mn1—C12 | 2.112 (7) |
Pt1—P1 | 2.3312 (16) | Mn1—C13 | 2.137 (7) |
Pt1—P2 | 2.2796 (17) | Mn1—C14 | 2.178 (7) |
Pt1—C1 | 1.991 (6) | Mn1—C15 | 2.146 (7) |
Pt1—C3 | 2.212 (7) | O3—C3 | 1.189 (8) |
Mn1—C1 | 1.924 (7) | O4—C4 | 1.153 (8) |
Mn1—C3 | 1.826 (7) | C1—C2 | 1.363 (9) |
Mn1—C4 | 1.775 (8) | C2—C5 | 1.469 (9) |
Mn1—C11 | 2.126 (7) | ||
C1—Pt1—C3 | 89.1 (3) | C4—Mn1—C1 | 92.4 (3) |
C1—Pt1—P2 | 102.7 (2) | C3—Mn1—C1 | 103.8 (3) |
C3—Pt1—P2 | 166.9 (2) | C2—C1—Mn1 | 143.2 (5) |
C1—Pt1—P1 | 169.4 (2) | C2—C1—Pt1 | 132.5 (5) |
C3—Pt1—P1 | 96.47 (19) | Mn1—C1—Pt1 | 83.5 (2) |
P2—Pt1—P1 | 72.83 (6) | C1—C2—C5 | 126.5 (6) |
C1—Pt1—Mn1 | 47.17 (19) | O3—C3—Mn1 | 153.4 (6) |
C3—Pt1—Mn1 | 43.57 (19) | O3—C3—Pt1 | 126.7 (5) |
P2—Pt1—Mn1 | 149.17 (5) | Mn1—C3—Pt1 | 79.8 (3) |
P1—Pt1—Mn1 | 135.32 (5) | O4—C4—Mn1 | 176.3 (6) |
C4—Mn1—C3 | 90.8 (3) | P2—C16—P1 | 95.9 (3) |
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