Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101013130/fr1342sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101013130/fr1342Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101013130/fr1342IIsup3.hkl |
CCDC references: 175076; 175077
For related literature, see: Altomare et al. (1994); Colton & Commons (1975); Hoskins & Steen (1983); Janke et al. (1986).
The title compounds were prepared according to the method of Colton & Commons (1975). Compound (I) was recrystallized from ethanol and (II) from toluene by evaporation under N2. Axial photographs of (II) confirmed that the Laue symmetry is 4/mmm.
Cell-reduction calculations for (I), and examination of the atomic coordinates and extended packing diagrams, failed to show any overlooked symmetry elements relating the two independent molecules. For both compounds, a SIR92 electron-density map (Altomare et al., 1994) showed all non-H atoms, and refinement was on F2 with net negative intensities reset at zero. H atoms [other than those of the toluene methyl group in (II)] were included at calculated positions, with C—H = 0.95 Å and Uiso(H) = 1.2Ueq(C). Refinement of the structure of (II) of opposite polarity (x,y,z → x,1/2 + y,-z) converged to slightly greater residuals [R(F) 0.048, I>σ(I), and wR(F2) 0.083, goodness of fit 1.39, all data].
For both compounds, data collection: CAD-4-PC Software (Enraf-Nonius, 1993); cell refinement: CAD-4-PC Software; data reduction: TEXSAN (Molecular Structure Corporation, 1997); program(s) used to solve structure: TEXSAN; program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.
[Mn2(CO)8(C25H22P2)] | Z = 4 |
Mr = 718.36 | F(000) = 1456.00 |
Triclinic, P1 | Dx = 1.493 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.6428 (13) Å | Cell parameters from 25 reflections |
b = 15.351 (4) Å | θ = 12.6–13.9° |
c = 17.868 (8) Å | µ = 0.94 mm−1 |
α = 111.91 (3)° | T = 296 K |
β = 94.05 (3)° | Plate, yellow |
γ = 90.48 (2)° | 0.40 × 0.20 × 0.05 mm |
V = 3207 (2) Å3 |
Enraf-Nonius CAD-4 diffractometer | 8260 reflections with I > σ(I) |
Radiation source: sealed X-ray tube | Rint = 0.021 |
Graphite monochromator | θmax = 25.0°, θmin = 1.5° |
ω/2θ scans | h = 0→15 |
Absorption correction: analytical (de Meulenaer & Tompa, 1965) | k = −18→18 |
Tmin = 0.763, Tmax = 0.958 | l = −21→21 |
11815 measured reflections | 3 standard reflections every 60 min |
11243 independent reflections | intensity decay: 4.5% |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.041 | w = 4Fo2/[σ2(I) + (0.02I)2] |
wR(F2) = 0.044 | (Δ/σ)max = 0.025 |
S = 1.40 | Δρmax = 0.47 e Å−3 |
11243 reflections | Δρmin = −0.46 e Å−3 |
811 parameters |
[Mn2(CO)8(C25H22P2)] | γ = 90.48 (2)° |
Mr = 718.36 | V = 3207 (2) Å3 |
Triclinic, P1 | Z = 4 |
a = 12.6428 (13) Å | Mo Kα radiation |
b = 15.351 (4) Å | µ = 0.94 mm−1 |
c = 17.868 (8) Å | T = 296 K |
α = 111.91 (3)° | 0.40 × 0.20 × 0.05 mm |
β = 94.05 (3)° |
Enraf-Nonius CAD-4 diffractometer | 8260 reflections with I > σ(I) |
Absorption correction: analytical (de Meulenaer & Tompa, 1965) | Rint = 0.021 |
Tmin = 0.763, Tmax = 0.958 | 3 standard reflections every 60 min |
11815 measured reflections | intensity decay: 4.5% |
11243 independent reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.044 | H-atom parameters constrained |
S = 1.40 | Δρmax = 0.47 e Å−3 |
11243 reflections | Δρmin = −0.46 e Å−3 |
811 parameters |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.63360 (4) | 0.57371 (3) | 0.80651 (3) | 0.04516 (14) | |
Mn2 | 0.44401 (4) | 0.65114 (3) | 0.74851 (3) | 0.04396 (14) | |
Mn3 | −0.08395 (4) | 0.06356 (3) | 0.80698 (3) | 0.04845 (15) | |
Mn4 | 0.09363 (4) | 0.14851 (3) | 0.75367 (3) | 0.04508 (14) | |
P1 | 0.57609 (6) | 0.42131 (6) | 0.73063 (5) | 0.0400 (2) | |
P2 | 0.35764 (6) | 0.51136 (6) | 0.73066 (5) | 0.0400 (2) | |
P3 | −0.04169 (6) | −0.08571 (6) | 0.72499 (5) | 0.0403 (2) | |
P4 | 0.17740 (6) | 0.00971 (6) | 0.73295 (5) | 0.0413 (2) | |
O1 | 0.8332 (2) | 0.5116 (2) | 0.86144 (17) | 0.0808 (10) | |
O2 | 0.6966 (2) | 0.7728 (2) | 0.90398 (19) | 0.0961 (11) | |
O3 | 0.5216 (2) | 0.57678 (19) | 0.94876 (15) | 0.0709 (9) | |
O4 | 0.7370 (2) | 0.5905 (2) | 0.66782 (17) | 0.0805 (10) | |
O5 | 0.2512 (2) | 0.72442 (18) | 0.69519 (15) | 0.0703 (9) | |
O6 | 0.5637 (3) | 0.8247 (2) | 0.76701 (19) | 0.0966 (12) | |
O7 | 0.4136 (2) | 0.74067 (18) | 0.92422 (15) | 0.0736 (9) | |
O8 | 0.5188 (2) | 0.57306 (19) | 0.58306 (15) | 0.0709 (9) | |
O9 | −0.2759 (2) | −0.0019 (2) | 0.85668 (19) | 0.0961 (12) | |
O10 | −0.1215 (3) | 0.2597 (2) | 0.9120 (2) | 0.1146 (12) | |
O11 | 0.0505 (2) | 0.0583 (2) | 0.94934 (16) | 0.0793 (10) | |
O12 | −0.2142 (2) | 0.0886 (2) | 0.67140 (18) | 0.0861 (11) | |
O13 | 0.2786 (2) | 0.22626 (18) | 0.70636 (16) | 0.0738 (9) | |
O14 | −0.0223 (3) | 0.3214 (2) | 0.77422 (19) | 0.1001 (12) | |
O15 | 0.1545 (2) | 0.23252 (18) | 0.93124 (16) | 0.0758 (9) | |
O16 | −0.0099 (2) | 0.07432 (19) | 0.58648 (15) | 0.0708 (9) | |
C1 | 0.7539 (3) | 0.5345 (3) | 0.8402 (2) | 0.0561 (11) | |
C2 | 0.6713 (3) | 0.6973 (3) | 0.8654 (2) | 0.0639 (12) | |
C3 | 0.5602 (3) | 0.5741 (2) | 0.8922 (2) | 0.0535 (11) | |
C4 | 0.6935 (3) | 0.5831 (2) | 0.7188 (2) | 0.0542 (11) | |
C5 | 0.3255 (3) | 0.6950 (2) | 0.71693 (19) | 0.0499 (10) | |
C6 | 0.5198 (3) | 0.7573 (3) | 0.7612 (2) | 0.0627 (12) | |
C7 | 0.4255 (3) | 0.7022 (2) | 0.8576 (2) | 0.0516 (10) | |
C8 | 0.4917 (3) | 0.5992 (2) | 0.6477 (2) | 0.0498 (10) | |
C9 | −0.1992 (3) | 0.0217 (3) | 0.8372 (2) | 0.0641 (12) | |
C10 | −0.1065 (3) | 0.1844 (3) | 0.8704 (3) | 0.0733 (13) | |
C11 | 0.0030 (3) | 0.0579 (2) | 0.8923 (2) | 0.0579 (11) | |
C12 | −0.1605 (3) | 0.0788 (3) | 0.7218 (2) | 0.0597 (12) | |
C13 | 0.2067 (3) | 0.1959 (2) | 0.7259 (2) | 0.0520 (10) | |
C14 | 0.0204 (3) | 0.2542 (3) | 0.7672 (2) | 0.0637 (12) | |
C15 | 0.1316 (3) | 0.1960 (2) | 0.8640 (2) | 0.0555 (11) | |
C16 | 0.0282 (3) | 0.0987 (2) | 0.6515 (2) | 0.0515 (11) | |
C17 | 0.4378 (2) | 0.4082 (2) | 0.68657 (17) | 0.0420 (9) | |
C18 | 0.5793 (2) | 0.3338 (2) | 0.7781 (2) | 0.0461 (10) | |
C19 | 0.5451 (3) | 0.2422 (3) | 0.7325 (2) | 0.0614 (12) | |
C20 | 0.5455 (3) | 0.1747 (3) | 0.7671 (3) | 0.0775 (15) | |
C21 | 0.5802 (3) | 0.1988 (4) | 0.8464 (3) | 0.0836 (18) | |
C22 | 0.6154 (3) | 0.2882 (4) | 0.8920 (3) | 0.0772 (16) | |
C23 | 0.6156 (3) | 0.3565 (3) | 0.8585 (2) | 0.0579 (11) | |
C24 | 0.6514 (2) | 0.3614 (2) | 0.64272 (18) | 0.0451 (9) | |
C25 | 0.7421 (3) | 0.3159 (3) | 0.6536 (2) | 0.0603 (12) | |
C26 | 0.8032 (3) | 0.2729 (3) | 0.5895 (3) | 0.0733 (14) | |
C27 | 0.7760 (4) | 0.2763 (3) | 0.5158 (3) | 0.0766 (14) | |
C28 | 0.6879 (4) | 0.3210 (3) | 0.5041 (2) | 0.0798 (15) | |
C29 | 0.6261 (3) | 0.3641 (3) | 0.5676 (2) | 0.0646 (12) | |
C30 | 0.3036 (2) | 0.5020 (2) | 0.81872 (18) | 0.0461 (9) | |
C31 | 0.3279 (3) | 0.4316 (3) | 0.8475 (2) | 0.0576 (11) | |
C32 | 0.2781 (3) | 0.4269 (4) | 0.9125 (3) | 0.0814 (16) | |
C33 | 0.2046 (4) | 0.4911 (5) | 0.9482 (3) | 0.0942 (18) | |
C34 | 0.1807 (3) | 0.5610 (4) | 0.9212 (3) | 0.0876 (16) | |
C35 | 0.2305 (3) | 0.5672 (3) | 0.8573 (2) | 0.0630 (12) | |
C36 | 0.2413 (2) | 0.4741 (2) | 0.65634 (18) | 0.0446 (9) | |
C37 | 0.1527 (3) | 0.4305 (3) | 0.6687 (2) | 0.0598 (11) | |
C38 | 0.0677 (3) | 0.4019 (3) | 0.6108 (3) | 0.0770 (14) | |
C39 | 0.0711 (3) | 0.4141 (3) | 0.5396 (3) | 0.0762 (14) | |
C40 | 0.1593 (3) | 0.4558 (3) | 0.5251 (2) | 0.0774 (14) | |
C41 | 0.2443 (3) | 0.4863 (3) | 0.5832 (2) | 0.0633 (12) | |
C42 | 0.0885 (2) | −0.0935 (2) | 0.68320 (17) | 0.0420 (9) | |
C43 | −0.0368 (2) | −0.1802 (2) | 0.76440 (19) | 0.0454 (9) | |
C44 | −0.0581 (3) | −0.1674 (3) | 0.8425 (2) | 0.0614 (12) | |
C45 | −0.0510 (3) | −0.2423 (3) | 0.8682 (3) | 0.0772 (15) | |
C46 | −0.0227 (3) | −0.3276 (3) | 0.8177 (3) | 0.0796 (16) | |
C47 | −0.0022 (3) | −0.3421 (3) | 0.7403 (3) | 0.0742 (14) | |
C48 | −0.0095 (3) | −0.2690 (2) | 0.7131 (2) | 0.0574 (11) | |
C49 | −0.1348 (2) | −0.1410 (2) | 0.63565 (19) | 0.0456 (9) | |
C50 | −0.2265 (3) | −0.1839 (3) | 0.6448 (2) | 0.0637 (12) | |
C51 | −0.3025 (3) | −0.2236 (3) | 0.5811 (3) | 0.0776 (14) | |
C52 | −0.2884 (4) | −0.2196 (3) | 0.5078 (3) | 0.0783 (14) | |
C53 | −0.1988 (4) | −0.1769 (3) | 0.4977 (2) | 0.0802 (15) | |
C54 | −0.1213 (3) | −0.1375 (3) | 0.5608 (2) | 0.0650 (12) | |
C55 | 0.2442 (2) | −0.0030 (2) | 0.82202 (18) | 0.0472 (10) | |
C56 | 0.3229 (3) | 0.0649 (3) | 0.8657 (2) | 0.0617 (12) | |
C57 | 0.3755 (3) | 0.0608 (3) | 0.9344 (3) | 0.0799 (14) | |
C58 | 0.3504 (4) | −0.0104 (4) | 0.9597 (3) | 0.0872 (17) | |
C59 | 0.2736 (3) | −0.0773 (3) | 0.9182 (3) | 0.0786 (16) | |
C60 | 0.2212 (3) | −0.0751 (3) | 0.8473 (2) | 0.0596 (12) | |
C61 | 0.2811 (2) | −0.0215 (2) | 0.66161 (19) | 0.0464 (10) | |
C62 | 0.2641 (3) | −0.0103 (3) | 0.5880 (2) | 0.0650 (12) | |
C63 | 0.3388 (4) | −0.0358 (3) | 0.5316 (2) | 0.0780 (15) | |
C64 | 0.4313 (4) | −0.0729 (3) | 0.5481 (3) | 0.0834 (16) | |
C65 | 0.4504 (3) | −0.0839 (3) | 0.6200 (3) | 0.0813 (15) | |
C66 | 0.3754 (3) | −0.0592 (3) | 0.6767 (2) | 0.0630 (12) | |
H1 | 0.4389 | 0.3953 | 0.6303 | 0.050* | |
H2 | 0.4047 | 0.3565 | 0.6940 | 0.050* | |
H3 | 0.5212 | 0.2253 | 0.6771 | 0.074* | |
H4 | 0.5217 | 0.1119 | 0.7355 | 0.093* | |
H5 | 0.5797 | 0.1528 | 0.8702 | 0.100* | |
H6 | 0.6401 | 0.3040 | 0.9471 | 0.093* | |
H7 | 0.6405 | 0.4188 | 0.8906 | 0.070* | |
H8 | 0.7623 | 0.3143 | 0.7052 | 0.072* | |
H9 | 0.8645 | 0.2409 | 0.5971 | 0.088* | |
H10 | 0.8189 | 0.2473 | 0.4722 | 0.092* | |
H11 | 0.6687 | 0.3226 | 0.4523 | 0.096* | |
H12 | 0.5652 | 0.3961 | 0.5592 | 0.078* | |
H13 | 0.3786 | 0.3867 | 0.8227 | 0.069* | |
H14 | 0.2950 | 0.3789 | 0.9323 | 0.098* | |
H15 | 0.1699 | 0.4867 | 0.9922 | 0.113* | |
H16 | 0.1298 | 0.6055 | 0.9464 | 0.105* | |
H17 | 0.2145 | 0.6169 | 0.8394 | 0.076* | |
H18 | 0.1497 | 0.4198 | 0.7176 | 0.072* | |
H19 | 0.0062 | 0.3734 | 0.6210 | 0.092* | |
H20 | 0.0126 | 0.3938 | 0.5000 | 0.091* | |
H21 | 0.1622 | 0.4639 | 0.4751 | 0.093* | |
H22 | 0.3050 | 0.5157 | 0.5729 | 0.076* | |
H23 | 0.1225 | −0.1464 | 0.6879 | 0.050* | |
H24 | 0.0770 | −0.1025 | 0.6277 | 0.050* | |
H25 | −0.0776 | −0.1076 | 0.8785 | 0.074* | |
H26 | −0.0662 | −0.2334 | 0.9218 | 0.093* | |
H27 | −0.0171 | −0.3779 | 0.8364 | 0.095* | |
H28 | 0.0170 | −0.4024 | 0.7051 | 0.089* | |
H29 | 0.0042 | −0.2795 | 0.6589 | 0.069* | |
H30 | −0.2377 | −0.1864 | 0.6960 | 0.076* | |
H31 | −0.3646 | −0.2536 | 0.5885 | 0.093* | |
H32 | −0.3407 | −0.2464 | 0.4640 | 0.094* | |
H33 | −0.1891 | −0.1741 | 0.4464 | 0.096* | |
H34 | −0.0591 | −0.1082 | 0.5526 | 0.078* | |
H35 | 0.3401 | 0.1141 | 0.8481 | 0.074* | |
H36 | 0.4290 | 0.1070 | 0.9641 | 0.096* | |
H37 | 0.3871 | −0.0131 | 1.0070 | 0.105* | |
H38 | 0.2558 | −0.1251 | 0.9373 | 0.094* | |
H39 | 0.1700 | −0.1232 | 0.8167 | 0.071* | |
H40 | 0.1999 | 0.0154 | 0.5763 | 0.078* | |
H41 | 0.3260 | −0.0276 | 0.4817 | 0.094* | |
H42 | 0.4826 | −0.0911 | 0.5093 | 0.100* | |
H43 | 0.5154 | −0.1087 | 0.6314 | 0.098* | |
H44 | 0.3890 | −0.0682 | 0.7262 | 0.076* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0455 (3) | 0.0485 (3) | 0.0396 (3) | 0.0002 (2) | −0.0017 (2) | 0.0153 (2) |
Mn2 | 0.0493 (3) | 0.0428 (3) | 0.0413 (3) | 0.0022 (2) | 0.0013 (2) | 0.0179 (2) |
Mn3 | 0.0525 (3) | 0.0465 (3) | 0.0431 (3) | 0.0072 (2) | 0.0147 (2) | 0.0110 (2) |
Mn4 | 0.0518 (3) | 0.0411 (3) | 0.0435 (3) | 0.0050 (2) | 0.0059 (2) | 0.0166 (2) |
P1 | 0.0417 (4) | 0.0449 (5) | 0.0351 (4) | 0.0037 (4) | 0.0024 (3) | 0.0171 (4) |
P2 | 0.0414 (4) | 0.0427 (5) | 0.0366 (4) | 0.0027 (4) | 0.0001 (3) | 0.0160 (4) |
P3 | 0.0454 (5) | 0.0415 (5) | 0.0346 (4) | 0.0029 (4) | 0.0083 (3) | 0.0142 (4) |
P4 | 0.0444 (4) | 0.0424 (5) | 0.0392 (5) | 0.0038 (4) | 0.0077 (4) | 0.0169 (4) |
O1 | 0.0521 (16) | 0.118 (2) | 0.094 (2) | 0.0061 (15) | −0.0038 (14) | 0.0663 (19) |
O2 | 0.090 (2) | 0.0612 (19) | 0.103 (2) | −0.0116 (16) | −0.0142 (17) | −0.0046 (17) |
O3 | 0.0735 (17) | 0.098 (2) | 0.0443 (15) | 0.0142 (14) | 0.0128 (13) | 0.0283 (15) |
O4 | 0.0777 (19) | 0.106 (2) | 0.0714 (19) | −0.0118 (16) | 0.0138 (15) | 0.0479 (17) |
O5 | 0.0696 (17) | 0.0767 (18) | 0.0698 (18) | 0.0266 (14) | 0.0060 (13) | 0.0330 (15) |
O6 | 0.112 (2) | 0.077 (2) | 0.108 (3) | −0.0340 (18) | −0.0061 (19) | 0.0458 (19) |
O7 | 0.102 (2) | 0.0667 (17) | 0.0443 (15) | 0.0144 (15) | 0.0044 (14) | 0.0122 (13) |
O8 | 0.0802 (18) | 0.0849 (19) | 0.0475 (16) | 0.0113 (14) | 0.0109 (13) | 0.0236 (14) |
O9 | 0.080 (2) | 0.104 (2) | 0.109 (3) | −0.0028 (17) | 0.0463 (18) | 0.039 (2) |
O10 | 0.113 (3) | 0.066 (2) | 0.123 (3) | 0.0225 (18) | 0.037 (2) | −0.0175 (19) |
O11 | 0.097 (2) | 0.090 (2) | 0.0460 (16) | −0.0009 (16) | 0.0008 (15) | 0.0215 (15) |
O12 | 0.080 (2) | 0.103 (2) | 0.085 (2) | 0.0263 (17) | 0.0028 (16) | 0.0472 (19) |
O13 | 0.0745 (18) | 0.0730 (18) | 0.0761 (19) | −0.0204 (14) | 0.0061 (14) | 0.0308 (15) |
O14 | 0.124 (3) | 0.075 (2) | 0.105 (3) | 0.0461 (19) | 0.0145 (19) | 0.0359 (18) |
O15 | 0.104 (2) | 0.0704 (18) | 0.0448 (16) | −0.0045 (15) | 0.0028 (14) | 0.0130 (14) |
O16 | 0.0797 (18) | 0.0833 (19) | 0.0473 (16) | 0.0035 (14) | −0.0026 (13) | 0.0235 (14) |
C1 | 0.053 (2) | 0.072 (3) | 0.049 (2) | −0.0061 (18) | 0.0022 (16) | 0.0292 (19) |
C2 | 0.057 (2) | 0.062 (3) | 0.058 (2) | 0.0046 (19) | −0.0050 (18) | 0.008 (2) |
C3 | 0.051 (2) | 0.060 (2) | 0.046 (2) | 0.0063 (16) | −0.0040 (16) | 0.0172 (18) |
C4 | 0.053 (2) | 0.057 (2) | 0.053 (2) | −0.0051 (16) | −0.0005 (17) | 0.0218 (18) |
C5 | 0.062 (2) | 0.048 (2) | 0.0402 (19) | 0.0054 (16) | 0.0085 (16) | 0.0155 (16) |
C6 | 0.072 (3) | 0.062 (3) | 0.058 (2) | −0.002 (2) | 0.0010 (19) | 0.027 (2) |
C7 | 0.063 (2) | 0.0426 (19) | 0.048 (2) | 0.0018 (16) | −0.0020 (17) | 0.0164 (17) |
C8 | 0.0502 (19) | 0.049 (2) | 0.053 (2) | 0.0042 (15) | 0.0021 (16) | 0.0221 (17) |
C9 | 0.069 (3) | 0.064 (2) | 0.059 (2) | 0.0087 (19) | 0.0226 (19) | 0.0181 (19) |
C10 | 0.067 (3) | 0.065 (3) | 0.074 (3) | 0.010 (2) | 0.021 (2) | 0.007 (2) |
C11 | 0.066 (2) | 0.056 (2) | 0.045 (2) | 0.0001 (17) | 0.0172 (18) | 0.0087 (18) |
C12 | 0.063 (2) | 0.054 (2) | 0.064 (3) | 0.0166 (18) | 0.0173 (19) | 0.0211 (19) |
C13 | 0.062 (2) | 0.0437 (19) | 0.049 (2) | −0.0027 (16) | −0.0021 (17) | 0.0175 (16) |
C14 | 0.078 (3) | 0.057 (2) | 0.055 (2) | 0.013 (2) | 0.0071 (19) | 0.0195 (19) |
C15 | 0.064 (2) | 0.047 (2) | 0.058 (2) | 0.0057 (17) | 0.0119 (18) | 0.0209 (19) |
C16 | 0.056 (2) | 0.046 (2) | 0.054 (2) | 0.0072 (16) | 0.0100 (17) | 0.0195 (17) |
C17 | 0.0440 (17) | 0.0445 (18) | 0.0348 (17) | 0.0022 (14) | −0.0005 (13) | 0.0123 (14) |
C18 | 0.0406 (17) | 0.054 (2) | 0.053 (2) | 0.0090 (15) | 0.0091 (15) | 0.0302 (17) |
C19 | 0.062 (2) | 0.057 (2) | 0.072 (3) | 0.0046 (18) | 0.0053 (19) | 0.032 (2) |
C20 | 0.077 (3) | 0.061 (3) | 0.107 (4) | 0.000 (2) | 0.008 (3) | 0.045 (3) |
C21 | 0.071 (3) | 0.100 (4) | 0.119 (4) | 0.016 (3) | 0.023 (3) | 0.083 (4) |
C22 | 0.076 (3) | 0.105 (4) | 0.075 (3) | 0.017 (3) | 0.012 (2) | 0.061 (3) |
C23 | 0.059 (2) | 0.074 (3) | 0.054 (2) | 0.0100 (18) | 0.0059 (17) | 0.038 (2) |
C24 | 0.0463 (18) | 0.0477 (19) | 0.0412 (18) | 0.0040 (15) | 0.0082 (14) | 0.0156 (15) |
C25 | 0.053 (2) | 0.075 (3) | 0.059 (2) | 0.0095 (18) | 0.0092 (17) | 0.030 (2) |
C26 | 0.059 (2) | 0.083 (3) | 0.082 (3) | 0.020 (2) | 0.024 (2) | 0.032 (3) |
C27 | 0.091 (3) | 0.067 (3) | 0.072 (3) | 0.016 (2) | 0.042 (2) | 0.019 (2) |
C28 | 0.117 (4) | 0.078 (3) | 0.052 (2) | 0.028 (3) | 0.034 (2) | 0.029 (2) |
C29 | 0.084 (3) | 0.066 (3) | 0.050 (2) | 0.028 (2) | 0.0193 (19) | 0.0255 (19) |
C30 | 0.0445 (18) | 0.056 (2) | 0.0362 (17) | −0.0061 (15) | −0.0017 (14) | 0.0161 (16) |
C31 | 0.055 (2) | 0.073 (3) | 0.051 (2) | −0.0124 (18) | −0.0063 (16) | 0.0311 (19) |
C32 | 0.073 (3) | 0.121 (4) | 0.070 (3) | −0.025 (3) | −0.011 (2) | 0.062 (3) |
C33 | 0.081 (3) | 0.156 (5) | 0.046 (3) | −0.025 (3) | 0.005 (2) | 0.039 (3) |
C34 | 0.077 (3) | 0.116 (4) | 0.053 (3) | 0.002 (3) | 0.020 (2) | 0.009 (3) |
C35 | 0.066 (2) | 0.068 (3) | 0.051 (2) | 0.0070 (19) | 0.0127 (18) | 0.0151 (19) |
C36 | 0.0440 (18) | 0.0417 (18) | 0.0452 (19) | 0.0064 (14) | −0.0039 (14) | 0.0143 (15) |
C37 | 0.057 (2) | 0.065 (2) | 0.057 (2) | −0.0045 (18) | −0.0073 (17) | 0.0245 (19) |
C38 | 0.057 (2) | 0.079 (3) | 0.087 (3) | −0.016 (2) | −0.014 (2) | 0.026 (3) |
C39 | 0.068 (3) | 0.079 (3) | 0.067 (3) | 0.002 (2) | −0.024 (2) | 0.016 (2) |
C40 | 0.082 (3) | 0.093 (3) | 0.053 (2) | 0.006 (2) | −0.016 (2) | 0.027 (2) |
C41 | 0.059 (2) | 0.081 (3) | 0.052 (2) | −0.0024 (19) | −0.0086 (17) | 0.029 (2) |
C42 | 0.0467 (18) | 0.0437 (18) | 0.0365 (17) | 0.0051 (14) | 0.0081 (13) | 0.0152 (14) |
C43 | 0.0418 (17) | 0.050 (2) | 0.048 (2) | −0.0029 (14) | 0.0013 (14) | 0.0238 (16) |
C44 | 0.071 (2) | 0.067 (2) | 0.052 (2) | −0.0031 (19) | 0.0072 (18) | 0.0291 (19) |
C45 | 0.084 (3) | 0.093 (3) | 0.077 (3) | −0.005 (3) | 0.005 (2) | 0.059 (3) |
C46 | 0.068 (3) | 0.082 (3) | 0.119 (4) | −0.003 (2) | 0.004 (3) | 0.073 (3) |
C47 | 0.071 (3) | 0.054 (2) | 0.107 (4) | 0.0054 (19) | 0.011 (2) | 0.040 (3) |
C48 | 0.063 (2) | 0.050 (2) | 0.063 (2) | 0.0008 (17) | 0.0095 (18) | 0.0243 (19) |
C49 | 0.0493 (19) | 0.0393 (18) | 0.0461 (19) | 0.0046 (14) | 0.0011 (15) | 0.0142 (15) |
C50 | 0.052 (2) | 0.078 (3) | 0.059 (2) | −0.0005 (19) | 0.0034 (17) | 0.023 (2) |
C51 | 0.058 (2) | 0.081 (3) | 0.084 (3) | −0.008 (2) | −0.011 (2) | 0.024 (3) |
C52 | 0.087 (3) | 0.061 (3) | 0.072 (3) | −0.005 (2) | −0.036 (2) | 0.015 (2) |
C53 | 0.114 (4) | 0.072 (3) | 0.051 (2) | −0.011 (3) | −0.019 (2) | 0.023 (2) |
C54 | 0.082 (3) | 0.064 (2) | 0.051 (2) | −0.014 (2) | −0.0077 (19) | 0.0272 (19) |
C55 | 0.0485 (19) | 0.054 (2) | 0.0389 (18) | 0.0120 (15) | 0.0076 (14) | 0.0160 (16) |
C56 | 0.061 (2) | 0.065 (2) | 0.053 (2) | 0.0030 (18) | −0.0012 (18) | 0.0162 (19) |
C57 | 0.068 (3) | 0.097 (3) | 0.058 (3) | 0.007 (2) | −0.012 (2) | 0.014 (2) |
C58 | 0.077 (3) | 0.135 (5) | 0.056 (3) | 0.026 (3) | −0.001 (2) | 0.044 (3) |
C59 | 0.076 (3) | 0.112 (4) | 0.070 (3) | 0.022 (3) | 0.012 (2) | 0.059 (3) |
C60 | 0.061 (2) | 0.068 (3) | 0.056 (2) | 0.0134 (18) | 0.0082 (17) | 0.031 (2) |
C61 | 0.0477 (19) | 0.0442 (18) | 0.049 (2) | 0.0017 (14) | 0.0145 (15) | 0.0176 (16) |
C62 | 0.063 (2) | 0.080 (3) | 0.060 (2) | 0.0113 (19) | 0.0193 (19) | 0.034 (2) |
C63 | 0.089 (3) | 0.092 (3) | 0.065 (3) | 0.011 (3) | 0.033 (2) | 0.039 (2) |
C64 | 0.081 (3) | 0.082 (3) | 0.095 (3) | 0.014 (2) | 0.050 (3) | 0.034 (3) |
C65 | 0.064 (3) | 0.091 (3) | 0.095 (3) | 0.028 (2) | 0.030 (2) | 0.038 (3) |
C66 | 0.060 (2) | 0.069 (3) | 0.065 (2) | 0.0151 (19) | 0.0197 (19) | 0.028 (2) |
Mn1—Mn2 | 2.9746 (7) | C28—C29 | 1.382 (5) |
Mn1—P1 | 2.3033 (9) | C28—H11 | 0.95 |
Mn1—C1 | 1.788 (4) | C29—H12 | 0.95 |
Mn1—C2 | 1.832 (4) | C30—C31 | 1.387 (4) |
Mn1—C3 | 1.844 (4) | C30—C35 | 1.387 (5) |
Mn1—C4 | 1.840 (4) | C31—C32 | 1.383 (5) |
Mn2—P2 | 2.3020 (9) | C31—H13 | 0.95 |
Mn2—C5 | 1.788 (4) | C32—C33 | 1.368 (7) |
Mn2—C6 | 1.814 (4) | C32—H14 | 0.95 |
Mn2—C7 | 1.842 (4) | C33—C34 | 1.359 (7) |
Mn2—C8 | 1.827 (4) | C33—H15 | 0.95 |
Mn3—Mn4 | 2.9714 (7) | C34—C35 | 1.374 (5) |
Mn3—P3 | 2.3039 (9) | C34—H16 | 0.95 |
Mn3—C9 | 1.784 (4) | C35—H17 | 0.95 |
Mn3—C10 | 1.815 (4) | C36—C37 | 1.373 (4) |
Mn3—C11 | 1.844 (4) | C36—C41 | 1.391 (4) |
Mn3—C12 | 1.836 (4) | C37—C38 | 1.383 (5) |
Mn4—P4 | 2.3028 (9) | C37—H18 | 0.95 |
Mn4—C13 | 1.781 (4) | C38—C39 | 1.357 (6) |
Mn4—C14 | 1.820 (4) | C38—H19 | 0.95 |
Mn4—C15 | 1.854 (4) | C39—C40 | 1.367 (6) |
Mn4—C16 | 1.827 (4) | C39—H20 | 0.95 |
P1—C17 | 1.844 (3) | C40—C41 | 1.386 (5) |
P1—C18 | 1.837 (3) | C40—H21 | 0.95 |
P1—C24 | 1.835 (3) | C41—H22 | 0.95 |
P2—C17 | 1.834 (3) | C42—H23 | 0.95 |
P2—C30 | 1.812 (3) | C42—H24 | 0.95 |
P2—C36 | 1.843 (3) | C43—C44 | 1.382 (4) |
P3—C42 | 1.842 (3) | C43—C48 | 1.392 (4) |
P3—C43 | 1.833 (3) | C44—C45 | 1.388 (5) |
P3—C49 | 1.833 (3) | C44—H25 | 0.95 |
P4—C42 | 1.828 (3) | C45—C46 | 1.353 (6) |
P4—C55 | 1.824 (3) | C45—H26 | 0.95 |
P4—C61 | 1.834 (3) | C46—C47 | 1.359 (6) |
O1—C1 | 1.150 (4) | C46—H27 | 0.95 |
O2—C2 | 1.135 (4) | C47—C48 | 1.381 (5) |
O3—C3 | 1.140 (4) | C47—H28 | 0.95 |
O4—C4 | 1.136 (4) | C48—H29 | 0.95 |
O5—C5 | 1.151 (4) | C49—C50 | 1.378 (5) |
O6—C6 | 1.137 (4) | C49—C54 | 1.381 (5) |
O7—C7 | 1.137 (4) | C50—C51 | 1.381 (5) |
O8—C8 | 1.150 (4) | C50—H30 | 0.95 |
O9—C9 | 1.153 (4) | C51—C52 | 1.357 (6) |
O10—C10 | 1.143 (4) | C51—H31 | 0.95 |
O11—C11 | 1.144 (4) | C52—C53 | 1.361 (6) |
O12—C12 | 1.145 (4) | C52—H32 | 0.95 |
O13—C13 | 1.151 (4) | C53—C54 | 1.386 (5) |
O14—C14 | 1.138 (4) | C53—H33 | 0.95 |
O15—C15 | 1.135 (4) | C54—H34 | 0.95 |
O16—C16 | 1.147 (4) | C55—C56 | 1.397 (5) |
C17—H1 | 0.95 | C55—C60 | 1.379 (5) |
C17—H2 | 0.95 | C56—C57 | 1.376 (5) |
C18—C19 | 1.383 (5) | C56—H35 | 0.95 |
C18—C23 | 1.388 (4) | C57—C58 | 1.372 (6) |
C19—C20 | 1.391 (5) | C57—H36 | 0.95 |
C19—H3 | 0.95 | C58—C59 | 1.363 (6) |
C20—C21 | 1.362 (6) | C58—H37 | 0.95 |
C20—H4 | 0.95 | C59—C60 | 1.399 (5) |
C21—C22 | 1.360 (6) | C59—H38 | 0.95 |
C21—H5 | 0.95 | C60—H39 | 0.95 |
C22—C23 | 1.387 (5) | C61—C62 | 1.390 (5) |
C22—H6 | 0.95 | C61—C66 | 1.382 (4) |
C23—H7 | 0.95 | C62—C63 | 1.381 (5) |
C24—C25 | 1.386 (4) | C62—H40 | 0.95 |
C24—C29 | 1.373 (4) | C63—C64 | 1.366 (6) |
C25—C26 | 1.383 (5) | C63—H41 | 0.95 |
C25—H8 | 0.95 | C64—C65 | 1.362 (6) |
C26—C27 | 1.358 (5) | C64—H42 | 0.95 |
C26—H9 | 0.95 | C65—C66 | 1.386 (5) |
C27—C28 | 1.357 (6) | C65—H43 | 0.95 |
C27—H10 | 0.95 | C66—H44 | 0.95 |
O1···O14i | 3.375 (4) | O6···C50ii | 3.526 (5) |
O1···C46ii | 3.405 (5) | O7···C59v | 3.352 (5) |
O1···C33iii | 3.484 (5) | O7···C22iii | 3.517 (5) |
O2···C57iii | 3.257 (5) | O8···O8iv | 2.980 (5) |
O2···C45ii | 3.292 (5) | O8···C29iv | 3.579 (4) |
O2···O15iii | 3.408 (4) | O9···C58vi | 3.416 (5) |
O2···C44ii | 3.585 (5) | O10···C34vii | 3.353 (5) |
O3···C22iii | 3.428 (5) | O10···C22viii | 3.370 (5) |
O3···C32iii | 3.433 (5) | O11···O11vi | 3.290 (6) |
O3···O3iii | 3.542 (5) | O11···C45vi | 3.425 (6) |
O4···C47ii | 3.458 (5) | O11···C44vi | 3.456 (4) |
O4···C40iv | 3.597 (5) | O13···C31 | 3.240 (4) |
O5···C60v | 3.305 (4) | O13···C19 | 3.363 (4) |
O5···C48v | 3.333 (4) | O13···C53ix | 3.506 (5) |
O5···C28iv | 3.508 (4) | O13···C17 | 3.566 (4) |
O5···C42v | 3.545 (4) | O14···C25viii | 3.533 (5) |
O5···C47v | 3.590 (5) | O15···C32 | 3.493 (5) |
O6···O9ii | 3.167 (4) | O16···O16ix | 3.111 (5) |
Mn2—Mn1—P1 | 92.17 (3) | C24—C25—H8 | 119.8 |
Mn2—Mn1—C1 | 175.32 (11) | C26—C25—H8 | 119.8 |
Mn2—Mn1—C2 | 84.37 (11) | C25—C26—C27 | 120.3 (4) |
Mn2—Mn1—C3 | 88.25 (10) | C25—C26—H9 | 119.9 |
Mn2—Mn1—C4 | 84.58 (10) | C27—C26—H9 | 119.9 |
P1—Mn1—C1 | 91.25 (12) | C26—C27—C28 | 120.3 (4) |
P1—Mn1—C2 | 176.48 (11) | C26—C27—H10 | 119.9 |
P1—Mn1—C3 | 91.39 (11) | C28—C27—H10 | 119.9 |
P1—Mn1—C4 | 90.70 (11) | C27—C28—C29 | 119.9 (4) |
C1—Mn1—C2 | 92.24 (16) | C27—C28—H11 | 120.0 |
C1—Mn1—C3 | 94.87 (14) | C29—C28—H11 | 120.0 |
C1—Mn1—C4 | 92.18 (15) | C24—C29—C28 | 121.1 (3) |
C2—Mn1—C3 | 87.89 (16) | C24—C29—H12 | 119.5 |
C2—Mn1—C4 | 89.60 (16) | C28—C29—H12 | 119.5 |
C3—Mn1—C4 | 172.60 (15) | P2—C30—C31 | 123.9 (3) |
Mn1—Mn2—P2 | 86.17 (3) | P2—C30—C35 | 117.6 (3) |
Mn1—Mn2—C5 | 176.71 (11) | C31—C30—C35 | 118.5 (3) |
Mn1—Mn2—C6 | 90.71 (12) | C30—C31—C32 | 119.9 (4) |
Mn1—Mn2—C7 | 82.06 (10) | C30—C31—H13 | 120.1 |
Mn1—Mn2—C8 | 86.63 (10) | C32—C31—H13 | 120.1 |
P2—Mn2—C5 | 91.40 (11) | C31—C32—C33 | 120.3 (4) |
P2—Mn2—C6 | 176.38 (12) | C31—C32—H14 | 119.9 |
P2—Mn2—C7 | 93.32 (11) | C33—C32—H14 | 119.9 |
P2—Mn2—C8 | 90.46 (10) | C32—C33—C34 | 120.6 (4) |
C5—Mn2—C6 | 91.79 (16) | C32—C33—H15 | 119.7 |
C5—Mn2—C7 | 95.89 (14) | C34—C33—H15 | 119.7 |
C5—Mn2—C8 | 95.61 (14) | C33—C34—C35 | 119.8 (4) |
C6—Mn2—C7 | 88.07 (16) | C33—C34—H16 | 120.1 |
C6—Mn2—C8 | 87.52 (16) | C35—C34—H16 | 120.1 |
C7—Mn2—C8 | 167.80 (14) | C30—C35—C34 | 121.0 (4) |
Mn4—Mn3—P3 | 91.58 (3) | C30—C35—H17 | 119.5 |
Mn4—Mn3—C9 | 173.93 (12) | C34—C35—H17 | 119.5 |
Mn4—Mn3—C10 | 83.89 (13) | P2—C36—C37 | 122.5 (3) |
Mn4—Mn3—C11 | 90.51 (11) | P2—C36—C41 | 119.4 (3) |
Mn4—Mn3—C12 | 83.80 (12) | C37—C36—C41 | 118.1 (3) |
P3—Mn3—C9 | 92.57 (12) | C36—C37—C38 | 120.8 (4) |
P3—Mn3—C10 | 175.30 (13) | C36—C37—H18 | 119.6 |
P3—Mn3—C11 | 91.51 (11) | C38—C37—H18 | 119.6 |
P3—Mn3—C12 | 90.80 (11) | C37—C38—C39 | 120.7 (4) |
C9—Mn3—C10 | 92.04 (17) | C37—C38—H19 | 119.6 |
C9—Mn3—C11 | 93.81 (16) | C39—C38—H19 | 119.6 |
C9—Mn3—C12 | 91.71 (17) | C38—C39—C40 | 119.7 (4) |
C10—Mn3—C11 | 87.27 (17) | C38—C39—H20 | 120.2 |
C10—Mn3—C12 | 89.98 (17) | C40—C39—H20 | 120.2 |
C11—Mn3—C12 | 173.92 (16) | C39—C40—C41 | 120.2 (4) |
Mn3—Mn4—P4 | 86.09 (3) | C39—C40—H21 | 119.9 |
Mn3—Mn4—C13 | 175.71 (11) | C41—C40—H21 | 119.9 |
Mn3—Mn4—C14 | 91.53 (12) | C36—C41—C40 | 120.5 (4) |
Mn3—Mn4—C15 | 81.11 (11) | C36—C41—H22 | 119.8 |
Mn3—Mn4—C16 | 87.43 (10) | C40—C41—H22 | 119.8 |
P4—Mn4—C13 | 90.75 (11) | P3—C42—P4 | 114.80 (16) |
P4—Mn4—C14 | 176.67 (12) | P3—C42—H23 | 108.1 |
P4—Mn4—C15 | 93.21 (10) | P3—C42—H24 | 108.1 |
P4—Mn4—C16 | 90.28 (10) | P4—C42—H23 | 108.1 |
C13—Mn4—C14 | 91.75 (16) | P4—C42—H24 | 108.1 |
C13—Mn4—C15 | 96.19 (15) | H23—C42—H24 | 109.5 |
C13—Mn4—C16 | 95.49 (15) | P3—C43—C44 | 123.3 (3) |
C14—Mn4—C15 | 88.71 (15) | P3—C43—C48 | 118.3 (3) |
C14—Mn4—C16 | 87.29 (15) | C44—C43—C48 | 118.4 (3) |
C15—Mn4—C16 | 167.76 (15) | C43—C44—C45 | 119.8 (4) |
Mn1—P1—C17 | 114.74 (10) | C43—C44—H25 | 120.1 |
Mn1—P1—C18 | 119.20 (11) | C45—C44—H25 | 120.1 |
Mn1—P1—C24 | 114.87 (10) | C44—C45—C46 | 120.7 (4) |
C17—P1—C18 | 102.14 (14) | C44—C45—H26 | 119.6 |
C17—P1—C24 | 103.41 (13) | C46—C45—H26 | 119.6 |
C18—P1—C24 | 100.17 (14) | C45—C46—C47 | 120.6 (4) |
Mn2—P2—C17 | 113.60 (10) | C45—C46—H27 | 119.7 |
Mn2—P2—C30 | 116.91 (11) | C47—C46—H27 | 119.7 |
Mn2—P2—C36 | 117.50 (10) | C46—C47—C48 | 119.9 (4) |
C17—P2—C30 | 107.07 (15) | C46—C47—H28 | 120.1 |
C17—P2—C36 | 98.35 (13) | C48—C47—H28 | 120.1 |
C30—P2—C36 | 101.11 (14) | C43—C48—C47 | 120.6 (4) |
Mn3—P3—C42 | 114.73 (10) | C43—C48—H29 | 119.7 |
Mn3—P3—C43 | 120.15 (11) | C47—C48—H29 | 119.7 |
Mn3—P3—C49 | 114.39 (10) | P3—C49—C50 | 118.1 (3) |
C42—P3—C43 | 101.61 (14) | P3—C49—C54 | 123.7 (3) |
C42—P3—C49 | 104.03 (14) | C50—C49—C54 | 118.0 (3) |
C43—P3—C49 | 99.53 (14) | C49—C50—C51 | 121.4 (4) |
Mn4—P4—C42 | 112.66 (10) | C49—C50—H30 | 119.3 |
Mn4—P4—C55 | 116.57 (11) | C51—C50—H30 | 119.3 |
Mn4—P4—C61 | 117.62 (11) | C50—C51—C52 | 120.0 (4) |
C42—P4—C55 | 107.26 (15) | C50—C51—H31 | 120.0 |
C42—P4—C61 | 98.58 (14) | C52—C51—H31 | 120.0 |
C55—P4—C61 | 102.10 (14) | C51—C52—C53 | 119.4 (4) |
Mn1—C1—O1 | 177.7 (3) | C51—C52—H32 | 120.3 |
Mn1—C2—O2 | 177.4 (4) | C53—C52—H32 | 120.3 |
Mn1—C3—O3 | 174.9 (3) | C52—C53—C54 | 121.3 (4) |
Mn1—C4—O4 | 175.3 (3) | C52—C53—H33 | 119.4 |
Mn2—C5—O5 | 177.8 (3) | C54—C53—H33 | 119.4 |
Mn2—C6—O6 | 176.9 (4) | C49—C54—C53 | 119.8 (4) |
Mn2—C7—O7 | 174.3 (3) | C49—C54—H34 | 120.1 |
Mn2—C8—O8 | 174.2 (3) | C53—C54—H34 | 120.1 |
Mn3—C9—O9 | 177.0 (4) | P4—C55—C56 | 116.9 (3) |
Mn3—C10—O10 | 178.2 (4) | P4—C55—C60 | 123.6 (3) |
Mn3—C11—O11 | 174.2 (3) | C56—C55—C60 | 119.5 (3) |
Mn3—C12—O12 | 175.4 (3) | C55—C56—C57 | 120.2 (4) |
Mn4—C13—O13 | 178.5 (3) | C55—C56—H35 | 119.9 |
Mn4—C14—O14 | 177.3 (4) | C57—C56—H35 | 119.9 |
Mn4—C15—O15 | 174.1 (3) | C56—C57—C58 | 119.7 (4) |
Mn4—C16—O16 | 174.0 (3) | C56—C57—H36 | 120.2 |
P1—C17—P2 | 114.82 (15) | C58—C57—H36 | 120.2 |
P1—C17—H1 | 108.1 | C57—C58—C59 | 121.1 (4) |
P1—C17—H2 | 108.1 | C57—C58—H37 | 119.4 |
P2—C17—H1 | 108.1 | C59—C58—H37 | 119.4 |
P2—C17—H2 | 108.1 | C58—C59—C60 | 119.8 (4) |
H1—C17—H2 | 109.5 | C58—C59—H38 | 120.1 |
P1—C18—C19 | 119.2 (3) | C60—C59—H38 | 120.1 |
P1—C18—C23 | 122.0 (3) | C55—C60—C59 | 119.6 (4) |
C19—C18—C23 | 118.8 (3) | C55—C60—H39 | 120.2 |
C18—C19—C20 | 120.5 (4) | C59—C60—H39 | 120.2 |
C18—C19—H3 | 119.8 | P4—C61—C62 | 119.6 (3) |
C20—C19—H3 | 119.8 | P4—C61—C66 | 122.5 (3) |
C19—C20—C21 | 119.8 (4) | C62—C61—C66 | 117.9 (3) |
C19—C20—H4 | 120.1 | C61—C62—C63 | 121.3 (4) |
C21—C20—H4 | 120.1 | C61—C62—H40 | 119.3 |
C20—C21—C22 | 120.6 (4) | C63—C62—H40 | 119.3 |
C20—C21—H5 | 119.7 | C62—C63—C64 | 119.6 (4) |
C22—C21—H5 | 119.7 | C62—C63—H41 | 120.2 |
C21—C22—C23 | 120.4 (4) | C64—C63—H41 | 120.2 |
C21—C22—H6 | 119.8 | C63—C64—C65 | 120.3 (4) |
C23—C22—H6 | 119.8 | C63—C64—H42 | 119.8 |
C18—C23—C22 | 120.0 (4) | C65—C64—H42 | 119.8 |
C18—C23—H7 | 120.0 | C64—C65—C66 | 120.4 (4) |
C22—C23—H7 | 120.0 | C64—C65—H43 | 119.8 |
P1—C24—C25 | 118.5 (2) | C66—C65—H43 | 119.8 |
P1—C24—C29 | 123.2 (3) | C61—C66—C65 | 120.5 (4) |
C25—C24—C29 | 118.1 (3) | C61—C66—H44 | 119.8 |
C24—C25—C26 | 120.3 (3) | C65—C66—H44 | 119.8 |
Mn1—Mn2—P2—C17 | −41.91 (10) | C10—Mn3—Mn4—C16 | −119.26 (17) |
Mn1—Mn2—P2—C30 | 83.61 (12) | C11—Mn3—Mn4—C13 | 20.5 (14) |
Mn1—Mn2—P2—C36 | −155.87 (11) | C11—Mn3—Mn4—C14 | −119.25 (16) |
Mn1—P1—C17—P2 | −15.44 (19) | C11—Mn3—Mn4—C15 | −30.79 (15) |
Mn1—P1—C18—C19 | −179.8 (2) | C11—Mn3—Mn4—C16 | 153.54 (15) |
Mn1—P1—C18—C23 | −0.1 (3) | C11—Mn3—P3—C42 | −77.90 (15) |
Mn1—P1—C24—C25 | 86.6 (3) | C11—Mn3—P3—C43 | 43.70 (16) |
Mn1—P1—C24—C29 | −89.2 (3) | C11—Mn3—P3—C49 | 161.97 (16) |
Mn2—Mn1—P1—C17 | −11.48 (11) | C12—Mn3—Mn4—C13 | −161.6 (14) |
Mn2—Mn1—P1—C18 | −133.00 (11) | C12—Mn3—Mn4—C14 | 58.59 (16) |
Mn2—Mn1—P1—C24 | 108.19 (11) | C12—Mn3—Mn4—C15 | 147.05 (15) |
Mn2—P2—C17—P1 | 44.50 (18) | C12—Mn3—Mn4—C16 | −28.62 (15) |
Mn2—P2—C30—C31 | −124.5 (3) | C12—Mn3—P3—C42 | 96.47 (16) |
Mn2—P2—C30—C35 | 58.2 (3) | C12—Mn3—P3—C43 | −141.93 (16) |
Mn2—P2—C36—C37 | −142.2 (3) | C12—Mn3—P3—C49 | −23.66 (16) |
Mn2—P2—C36—C41 | 40.8 (3) | C13—Mn4—P4—C42 | −139.33 (15) |
Mn3—Mn4—P4—C42 | 43.57 (10) | C13—Mn4—P4—C55 | 96.05 (16) |
Mn3—Mn4—P4—C55 | −81.05 (12) | C13—Mn4—P4—C61 | −25.70 (16) |
Mn3—Mn4—P4—C61 | 157.20 (12) | C14—Mn4—P4—C42 | −1 (2) |
Mn3—P3—C42—P4 | 15.34 (19) | C14—Mn4—P4—C55 | −125 (2) |
Mn3—P3—C43—C44 | 0.5 (3) | C14—Mn4—P4—C61 | 113 (2) |
Mn3—P3—C43—C48 | −179.2 (2) | C15—Mn4—P4—C42 | 124.43 (15) |
Mn3—P3—C49—C50 | −82.5 (3) | C15—Mn4—P4—C55 | −0.20 (16) |
Mn3—P3—C49—C54 | 93.7 (3) | C15—Mn4—P4—C61 | −121.94 (16) |
Mn4—Mn3—P3—C42 | 12.65 (11) | C16—Mn4—P4—C42 | −43.83 (15) |
Mn4—Mn3—P3—C43 | 134.25 (11) | C16—Mn4—P4—C55 | −168.46 (16) |
Mn4—Mn3—P3—C49 | −107.48 (12) | C16—Mn4—P4—C61 | 69.80 (16) |
Mn4—P4—C42—P3 | −45.73 (18) | C17—P1—C18—C19 | 52.6 (3) |
Mn4—P4—C55—C56 | −57.8 (3) | C17—P1—C18—C23 | −127.8 (3) |
Mn4—P4—C55—C60 | 122.4 (3) | C17—P1—C24—C25 | −147.6 (3) |
Mn4—P4—C61—C62 | −44.1 (3) | C17—P1—C24—C29 | 36.5 (3) |
Mn4—P4—C61—C66 | 138.2 (3) | C17—P2—C30—C31 | 4.2 (3) |
P1—Mn1—Mn2—P2 | 26.93 (3) | C17—P2—C30—C35 | −173.1 (3) |
P1—Mn1—Mn2—C6 | −151.23 (12) | C17—P2—C36—C37 | 95.7 (3) |
P1—Mn1—Mn2—C7 | 120.82 (11) | C17—P2—C36—C41 | −81.4 (3) |
P1—Mn1—Mn2—C8 | −63.76 (10) | C18—P1—C24—C25 | −42.4 (3) |
P1—C17—P2—C30 | −86.10 (18) | C18—P1—C24—C29 | 141.7 (3) |
P1—C17—P2—C36 | 169.49 (17) | C18—C19—C20—C21 | −0.2 (6) |
P1—C18—C19—C20 | −179.3 (3) | C18—C23—C22—C21 | 0.2 (6) |
P1—C18—C23—C22 | 179.3 (3) | C19—C18—P1—C24 | −53.7 (3) |
P1—C24—C25—C26 | −177.6 (3) | C19—C18—C23—C22 | −1.0 (5) |
P1—C24—C29—C28 | 177.3 (3) | C19—C20—C21—C22 | −0.7 (7) |
P2—Mn2—Mn1—C2 | −152.44 (13) | C20—C19—C18—C23 | 1.1 (5) |
P2—Mn2—Mn1—C3 | −64.40 (11) | C20—C21—C22—C23 | 0.7 (7) |
P2—Mn2—Mn1—C4 | 117.43 (11) | C23—C18—P1—C24 | 126.0 (3) |
P2—C17—P1—C18 | 115.00 (18) | C24—C25—C26—C27 | 1.2 (6) |
P2—C17—P1—C24 | −141.30 (17) | C24—C29—C28—C27 | −1.0 (7) |
P2—C30—C31—C32 | −176.3 (3) | C25—C24—C29—C28 | 1.4 (6) |
P2—C30—C35—C34 | 175.7 (3) | C25—C26—C27—C28 | −0.8 (7) |
P2—C36—C37—C38 | −178.8 (3) | C26—C25—C24—C29 | −1.5 (5) |
P2—C36—C41—C40 | 177.7 (3) | C26—C27—C28—C29 | 0.7 (7) |
P3—Mn3—Mn4—P4 | −28.44 (3) | C30—P2—C36—C37 | −13.7 (3) |
P3—Mn3—Mn4—C14 | 149.23 (12) | C30—P2—C36—C41 | 169.3 (3) |
P3—Mn3—Mn4—C15 | −122.31 (11) | C30—C31—C32—C33 | 0.3 (6) |
P3—Mn3—Mn4—C16 | 62.01 (10) | C30—C35—C34—C33 | 1.2 (6) |
P3—C42—P4—C55 | 83.85 (18) | C31—C30—P2—C36 | 106.6 (3) |
P3—C42—P4—C61 | −170.55 (17) | C31—C30—C35—C34 | −1.8 (5) |
P3—C43—C44—C45 | −179.0 (3) | C31—C32—C33—C34 | −1.0 (7) |
P3—C43—C48—C47 | 178.5 (3) | C32—C31—C30—C35 | 1.1 (5) |
P3—C49—C50—C51 | 177.2 (3) | C32—C33—C34—C35 | 0.2 (7) |
P3—C49—C54—C53 | −176.4 (3) | C35—C30—P2—C36 | −70.7 (3) |
P4—Mn4—Mn3—C9 | −161.6 (12) | C36—C37—C38—C39 | 1.7 (6) |
P4—Mn4—Mn3—C10 | 150.28 (14) | C36—C41—C40—C39 | 0.6 (6) |
P4—Mn4—Mn3—C11 | 63.08 (11) | C37—C36—C41—C40 | 0.6 (5) |
P4—Mn4—Mn3—C12 | −119.08 (11) | C37—C38—C39—C40 | −0.5 (7) |
P4—C42—P3—C43 | −115.90 (17) | C38—C37—C36—C41 | −1.7 (5) |
P4—C42—P3—C49 | 141.06 (16) | C38—C39—C40—C41 | −0.6 (7) |
P4—C55—C56—C57 | 178.9 (3) | C42—P3—C43—C44 | 128.3 (3) |
P4—C55—C60—C59 | −177.5 (3) | C42—P3—C43—C48 | −51.3 (3) |
P4—C61—C62—C63 | −177.9 (3) | C42—P3—C49—C50 | 151.5 (3) |
P4—C61—C66—C65 | 178.3 (3) | C42—P3—C49—C54 | −32.2 (3) |
C1—Mn1—P1—C17 | 171.72 (15) | C42—P4—C55—C56 | 174.9 (2) |
C1—Mn1—P1—C18 | 50.21 (15) | C42—P4—C55—C60 | −4.9 (3) |
C1—Mn1—P1—C24 | −68.61 (15) | C42—P4—C61—C62 | 77.2 (3) |
C2—Mn1—Mn2—C5 | −110.0 (18) | C42—P4—C61—C66 | −100.5 (3) |
C2—Mn1—Mn2—C6 | 29.40 (17) | C43—P3—C49—C50 | 46.9 (3) |
C2—Mn1—Mn2—C7 | −58.55 (16) | C43—P3—C49—C54 | −136.8 (3) |
C2—Mn1—Mn2—C8 | 116.87 (16) | C43—C44—C45—C46 | 0.4 (6) |
C3—Mn1—Mn2—C5 | −22.0 (18) | C43—C48—C47—C46 | 0.6 (6) |
C3—Mn1—Mn2—C6 | 117.45 (16) | C44—C43—P3—C49 | −125.1 (3) |
C3—Mn1—Mn2—C7 | 29.50 (15) | C44—C43—C48—C47 | −1.2 (5) |
C3—Mn1—Mn2—C8 | −155.08 (15) | C44—C45—C46—C47 | −1.0 (7) |
C3—Mn1—P1—C17 | 76.83 (15) | C45—C44—C43—C48 | 0.7 (5) |
C3—Mn1—P1—C18 | −44.69 (15) | C45—C46—C47—C48 | 0.5 (6) |
C3—Mn1—P1—C24 | −163.51 (15) | C48—C43—P3—C49 | 55.2 (3) |
C4—Mn1—Mn2—C5 | 159.8 (18) | C49—C50—C51—C52 | −0.9 (6) |
C4—Mn1—Mn2—C6 | −60.73 (16) | C49—C54—C53—C52 | −0.2 (6) |
C4—Mn1—Mn2—C7 | −148.67 (15) | C50—C49—C54—C53 | −0.2 (6) |
C4—Mn1—Mn2—C8 | 26.74 (15) | C50—C51—C52—C53 | 0.4 (7) |
C4—Mn1—P1—C17 | −96.08 (15) | C51—C50—C49—C54 | 0.8 (6) |
C4—Mn1—P1—C18 | 142.40 (15) | C51—C52—C53—C54 | 0.1 (7) |
C4—Mn1—P1—C24 | 23.59 (15) | C55—P4—C61—C62 | −173.0 (3) |
C5—Mn2—P2—C17 | 140.31 (14) | C55—P4—C61—C66 | 9.3 (3) |
C5—Mn2—P2—C30 | −94.17 (15) | C55—C56—C57—C58 | 0.0 (6) |
C5—Mn2—P2—C36 | 26.36 (15) | C55—C60—C59—C58 | −2.9 (6) |
C7—Mn2—P2—C17 | −123.71 (14) | C56—C55—P4—C61 | 71.8 (3) |
C7—Mn2—P2—C30 | 1.81 (15) | C56—C55—C60—C59 | 2.7 (5) |
C7—Mn2—P2—C36 | 122.34 (15) | C56—C57—C58—C59 | −0.2 (7) |
C8—Mn2—P2—C17 | 44.69 (14) | C57—C56—C55—C60 | −1.3 (5) |
C8—Mn2—P2—C30 | 170.20 (15) | C57—C58—C59—C60 | 1.7 (7) |
C8—Mn2—P2—C36 | −69.27 (15) | C60—C55—P4—C61 | −108.0 (3) |
C9—Mn3—P3—C42 | −171.78 (16) | C61—C62—C63—C64 | 0.1 (7) |
C9—Mn3—P3—C43 | −50.18 (17) | C61—C66—C65—C64 | −1.1 (7) |
C9—Mn3—P3—C49 | 68.09 (17) | C62—C61—C66—C65 | 0.6 (6) |
C10—Mn3—Mn4—C13 | 107.7 (14) | C62—C63—C64—C65 | −0.6 (7) |
C10—Mn3—Mn4—C14 | −32.05 (18) | C63—C62—C61—C66 | −0.1 (6) |
C10—Mn3—Mn4—C15 | 56.41 (17) | C63—C64—C65—C66 | 1.1 (7) |
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1, z; (iii) −x+1, −y+1, −z+2; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z; (vi) −x, −y, −z+2; (vii) −x, −y+1, −z+2; (viii) x−1, y, z; (ix) −x, −y, −z+1. |
[Mn2(CO)8(C25H22P2)]·0.5C7H8 | Dx = 1.469 Mg m−3 |
Mr = 764.43 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41cd | Cell parameters from 25 reflections |
Hall symbol: I 41b -2c | θ = 15.5–16.0° |
a = 18.286 (2) Å | µ = 0.87 mm−1 |
c = 41.345 (6) Å | T = 294 K |
V = 13824 (3) Å3 | Block, yellow |
Z = 16 | 0.36 × 0.32 × 0.29 mm |
F(000) = 6224.00 |
Enraf-Nonius CAD-4 diffractometer | 2520 reflections with I > 1σ(I) |
Radiation source: sealed X-ray tube | Rint = 0.000 |
Graphite monochromator | θmax = 25.0°, θmin = 1.6° |
ω scans | h = 0→21 |
Absorption correction: ψ-scan (North et al., 1968) | k = 0→15 |
Tmin = 0.72, Tmax = 0.77 | l = 0→49 |
3084 measured reflections | 3 standard reflections every 60 min |
3084 independent reflections | intensity decay: 1.1% |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | 0 constraints |
R[F2 > 2σ(F2)] = 0.045 | H-atom parameters constrained |
wR(F2) = 0.038 | w = 4Fo2/[σ2(I) + (0.02I)2] |
S = 1.32 | (Δ/σ)max = 0.005 |
3084 reflections | Δρmax = 0.48 e Å−3 |
438 parameters | Δρmin = −0.48 e Å−3 |
[Mn2(CO)8(C25H22P2)]·0.5C7H8 | Z = 16 |
Mr = 764.43 | Mo Kα radiation |
Tetragonal, I41cd | µ = 0.87 mm−1 |
a = 18.286 (2) Å | T = 294 K |
c = 41.345 (6) Å | 0.36 × 0.32 × 0.29 mm |
V = 13824 (3) Å3 |
Enraf-Nonius CAD-4 diffractometer | 2520 reflections with I > 1σ(I) |
Absorption correction: ψ-scan (North et al., 1968) | Rint = 0.000 |
Tmin = 0.72, Tmax = 0.77 | 3 standard reflections every 60 min |
3084 measured reflections | intensity decay: 1.1% |
3084 independent reflections |
R[F2 > 2σ(F2)] = 0.045 | 0 restraints |
wR(F2) = 0.038 | H-atom parameters constrained |
S = 1.32 | Δρmax = 0.48 e Å−3 |
3084 reflections | Δρmin = −0.48 e Å−3 |
438 parameters |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.68920 (5) | 0.64484 (5) | 0.5000 | 0.0407 (3) | |
Mn2 | 0.60238 (5) | 0.63975 (5) | 0.55966 (3) | 0.0423 (3) | |
P1 | 0.64564 (9) | 0.76189 (9) | 0.49097 (5) | 0.0368 (5) | |
P2 | 0.62335 (9) | 0.76355 (9) | 0.56508 (5) | 0.0372 (5) | |
O1 | 0.7646 (3) | 0.6396 (3) | 0.43734 (13) | 0.0691 (19) | |
O2 | 0.5559 (3) | 0.5771 (3) | 0.47107 (16) | 0.082 (2) | |
O3 | 0.7437 (3) | 0.4977 (3) | 0.51898 (14) | 0.0719 (18) | |
O4 | 0.8217 (3) | 0.6932 (3) | 0.53497 (13) | 0.0661 (19) | |
O5 | 0.4660 (3) | 0.6708 (3) | 0.52227 (13) | 0.0621 (18) | |
O6 | 0.5775 (3) | 0.4832 (3) | 0.5466 (2) | 0.100 (3) | |
O7 | 0.7452 (3) | 0.5935 (3) | 0.58729 (13) | 0.0612 (17) | |
O8 | 0.5286 (3) | 0.6288 (4) | 0.62228 (16) | 0.096 (2) | |
C1 | 0.7347 (4) | 0.6432 (4) | 0.46202 (18) | 0.047 (2) | |
C2 | 0.6059 (5) | 0.6045 (4) | 0.48308 (19) | 0.059 (3) | |
C3 | 0.7212 (4) | 0.5536 (4) | 0.51171 (18) | 0.051 (2) | |
C4 | 0.7675 (4) | 0.6781 (4) | 0.52275 (16) | 0.044 (2) | |
C5 | 0.5198 (5) | 0.6602 (4) | 0.53607 (18) | 0.051 (2) | |
C6 | 0.5877 (4) | 0.5436 (4) | 0.5513 (2) | 0.063 (3) | |
C7 | 0.6914 (4) | 0.6143 (4) | 0.57623 (18) | 0.046 (2) | |
C8 | 0.5571 (4) | 0.6344 (4) | 0.5978 (2) | 0.059 (3) | |
C9 | 0.6160 (4) | 0.8131 (4) | 0.52706 (17) | 0.047 (2) | |
C10 | 0.5679 (3) | 0.7658 (4) | 0.46352 (16) | 0.0386 (19) | |
C11 | 0.4998 (4) | 0.7940 (4) | 0.47055 (19) | 0.063 (2) | |
C12 | 0.4432 (5) | 0.7943 (6) | 0.4482 (3) | 0.084 (4) | |
C13 | 0.4556 (5) | 0.7673 (6) | 0.4180 (3) | 0.078 (3) | |
C14 | 0.5226 (5) | 0.7392 (6) | 0.4103 (2) | 0.077 (3) | |
C15 | 0.5774 (4) | 0.7376 (5) | 0.43250 (19) | 0.060 (3) | |
C16 | 0.5576 (4) | 0.8158 (4) | 0.58945 (16) | 0.0385 (19) | |
C17 | 0.5796 (4) | 0.8641 (4) | 0.61387 (18) | 0.052 (2) | |
C18 | 0.5284 (5) | 0.9045 (4) | 0.6310 (2) | 0.065 (3) | |
C19 | 0.4550 (5) | 0.8968 (5) | 0.6248 (2) | 0.062 (3) | |
C20 | 0.4335 (4) | 0.8496 (5) | 0.6013 (2) | 0.063 (3) | |
C21 | 0.4832 (4) | 0.8087 (4) | 0.58377 (19) | 0.057 (3) | |
C22 | 0.7101 (4) | 0.7896 (3) | 0.58353 (16) | 0.0378 (19) | |
C23 | 0.7266 (4) | 0.7578 (4) | 0.61303 (16) | 0.049 (2) | |
C24 | 0.7910 (5) | 0.7750 (5) | 0.62854 (19) | 0.065 (3) | |
C25 | 0.8398 (5) | 0.8220 (6) | 0.6148 (3) | 0.082 (4) | |
C26 | 0.8251 (5) | 0.8518 (5) | 0.5860 (3) | 0.078 (3) | |
C27 | 0.7605 (4) | 0.8378 (4) | 0.56902 (18) | 0.062 (3) | |
C28 | 0.7071 (4) | 0.8288 (4) | 0.47190 (16) | 0.0387 (19) | |
C29 | 0.7825 (4) | 0.8227 (4) | 0.4744 (2) | 0.062 (3) | |
C30 | 0.8276 (4) | 0.8761 (5) | 0.4616 (2) | 0.071 (3) | |
C31 | 0.7984 (6) | 0.9349 (5) | 0.4464 (2) | 0.069 (3) | |
C32 | 0.7240 (6) | 0.9407 (4) | 0.4428 (2) | 0.069 (3) | |
C33 | 0.6787 (4) | 0.8877 (4) | 0.45615 (18) | 0.050 (2) | |
C34 | 0.5000 | 0.5000 | 0.7941 (4) | 0.088 (5) | |
C35 | 0.4766 (5) | 0.4415 (5) | 0.7763 (3) | 0.090 (4) | |
C36 | 0.4762 (5) | 0.4399 (5) | 0.7431 (3) | 0.080 (3) | |
C37 | 0.5000 | 0.5000 | 0.7248 (4) | 0.075 (4) | |
C38 | 0.5000 | 0.5000 | 0.6887 (3) | 0.112 (6) | |
H1 | 0.6451 | 0.8559 | 0.5286 | 0.057* | |
H2 | 0.5662 | 0.8265 | 0.5241 | 0.057* | |
H3 | 0.4914 | 0.8140 | 0.4914 | 0.075* | |
H4 | 0.3965 | 0.8131 | 0.4539 | 0.100* | |
H5 | 0.4177 | 0.7679 | 0.4024 | 0.094* | |
H6 | 0.5309 | 0.7206 | 0.3891 | 0.093* | |
H7 | 0.6232 | 0.7168 | 0.4268 | 0.072* | |
H8 | 0.6301 | 0.8692 | 0.6187 | 0.062* | |
H9 | 0.5442 | 0.9377 | 0.6473 | 0.078* | |
H10 | 0.4198 | 0.9240 | 0.6366 | 0.074* | |
H11 | 0.3829 | 0.8445 | 0.5967 | 0.075* | |
H12 | 0.4664 | 0.7754 | 0.5678 | 0.068* | |
H13 | 0.6935 | 0.7241 | 0.6226 | 0.059* | |
H14 | 0.8014 | 0.7538 | 0.6490 | 0.078* | |
H15 | 0.8841 | 0.8336 | 0.6257 | 0.098* | |
H16 | 0.8600 | 0.8840 | 0.5767 | 0.094* | |
H17 | 0.7510 | 0.8597 | 0.5486 | 0.075* | |
H18 | 0.8033 | 0.7815 | 0.4850 | 0.074* | |
H19 | 0.8792 | 0.8715 | 0.4636 | 0.085* | |
H20 | 0.8294 | 0.9721 | 0.4381 | 0.082* | |
H21 | 0.7037 | 0.9807 | 0.4312 | 0.083* | |
H22 | 0.6271 | 0.8927 | 0.4543 | 0.060* | |
H23 | 0.5000 | 0.5000 | 0.8171 | 0.106* | |
H24 | 0.4595 | 0.3995 | 0.7875 | 0.108* | |
H26 | 0.4596 | 0.3973 | 0.7322 | 0.096* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0417 (6) | 0.0370 (6) | 0.0434 (6) | 0.0029 (5) | −0.0055 (5) | −0.0002 (5) |
Mn2 | 0.0394 (6) | 0.0388 (6) | 0.0489 (6) | −0.0045 (5) | −0.0027 (5) | 0.0064 (6) |
P1 | 0.0386 (10) | 0.0383 (10) | 0.0336 (9) | 0.0032 (8) | −0.0021 (8) | 0.0012 (8) |
P2 | 0.0394 (10) | 0.0402 (10) | 0.0321 (9) | −0.0021 (8) | −0.0030 (8) | 0.0041 (8) |
O1 | 0.072 (4) | 0.080 (4) | 0.055 (3) | 0.008 (3) | 0.013 (3) | −0.007 (3) |
O2 | 0.064 (4) | 0.085 (5) | 0.097 (5) | −0.015 (3) | −0.020 (4) | −0.017 (4) |
O3 | 0.095 (4) | 0.038 (3) | 0.083 (4) | 0.014 (3) | −0.007 (4) | 0.010 (3) |
O4 | 0.056 (3) | 0.071 (4) | 0.072 (4) | 0.002 (3) | −0.016 (3) | 0.003 (3) |
O5 | 0.054 (3) | 0.064 (4) | 0.068 (4) | 0.000 (3) | −0.017 (3) | 0.009 (3) |
O6 | 0.069 (4) | 0.034 (3) | 0.196 (8) | −0.013 (3) | −0.031 (5) | 0.008 (4) |
O7 | 0.054 (3) | 0.066 (4) | 0.063 (3) | 0.008 (3) | −0.011 (3) | 0.010 (3) |
O8 | 0.084 (5) | 0.131 (6) | 0.073 (4) | 0.013 (4) | 0.029 (4) | 0.043 (4) |
C1 | 0.047 (4) | 0.046 (4) | 0.048 (5) | 0.003 (4) | −0.011 (4) | −0.001 (4) |
C2 | 0.074 (6) | 0.040 (5) | 0.062 (6) | 0.010 (4) | −0.003 (5) | 0.002 (4) |
C3 | 0.055 (5) | 0.048 (5) | 0.049 (5) | −0.007 (4) | −0.009 (4) | 0.005 (4) |
C4 | 0.054 (5) | 0.041 (4) | 0.038 (4) | 0.010 (4) | −0.006 (4) | 0.006 (3) |
C5 | 0.057 (5) | 0.037 (4) | 0.058 (5) | −0.007 (4) | 0.001 (4) | 0.004 (4) |
C6 | 0.045 (5) | 0.052 (5) | 0.091 (7) | −0.006 (4) | −0.017 (5) | 0.019 (5) |
C7 | 0.045 (5) | 0.047 (4) | 0.045 (4) | −0.006 (4) | −0.005 (4) | 0.006 (4) |
C8 | 0.058 (5) | 0.050 (5) | 0.069 (6) | −0.002 (4) | −0.002 (5) | 0.016 (5) |
C9 | 0.063 (5) | 0.036 (4) | 0.043 (4) | 0.003 (4) | −0.002 (4) | 0.000 (3) |
C10 | 0.035 (4) | 0.045 (4) | 0.036 (4) | −0.005 (3) | −0.002 (3) | 0.005 (3) |
C11 | 0.043 (4) | 0.079 (5) | 0.066 (5) | 0.015 (4) | −0.003 (5) | 0.004 (5) |
C12 | 0.044 (5) | 0.118 (9) | 0.089 (7) | 0.019 (5) | −0.016 (5) | 0.005 (7) |
C13 | 0.056 (6) | 0.097 (7) | 0.082 (7) | −0.004 (5) | −0.035 (6) | 0.010 (6) |
C14 | 0.080 (7) | 0.106 (8) | 0.046 (5) | −0.001 (6) | −0.023 (5) | −0.008 (5) |
C15 | 0.050 (5) | 0.078 (6) | 0.052 (5) | 0.008 (4) | −0.006 (4) | −0.001 (5) |
C16 | 0.045 (4) | 0.039 (4) | 0.031 (4) | 0.004 (3) | 0.002 (3) | 0.003 (3) |
C17 | 0.050 (4) | 0.059 (5) | 0.047 (5) | −0.008 (4) | 0.000 (4) | 0.000 (4) |
C18 | 0.076 (6) | 0.053 (5) | 0.067 (6) | 0.003 (5) | 0.003 (5) | −0.018 (5) |
C19 | 0.063 (6) | 0.057 (5) | 0.065 (6) | 0.002 (5) | 0.016 (5) | 0.004 (5) |
C20 | 0.041 (4) | 0.061 (5) | 0.087 (6) | 0.002 (4) | −0.005 (5) | 0.011 (5) |
C21 | 0.052 (5) | 0.054 (5) | 0.064 (5) | 0.000 (4) | 0.000 (4) | −0.016 (4) |
C22 | 0.046 (4) | 0.035 (4) | 0.033 (4) | 0.000 (3) | 0.003 (3) | −0.009 (3) |
C23 | 0.049 (4) | 0.056 (5) | 0.041 (4) | 0.000 (4) | −0.003 (4) | −0.012 (4) |
C24 | 0.060 (5) | 0.078 (6) | 0.056 (6) | 0.000 (5) | −0.018 (4) | −0.015 (5) |
C25 | 0.054 (6) | 0.106 (8) | 0.085 (7) | −0.006 (6) | −0.019 (5) | −0.025 (7) |
C26 | 0.050 (5) | 0.092 (7) | 0.092 (7) | −0.036 (5) | 0.016 (5) | −0.005 (6) |
C27 | 0.067 (5) | 0.067 (5) | 0.053 (5) | −0.030 (4) | 0.014 (4) | −0.002 (4) |
C28 | 0.041 (4) | 0.037 (4) | 0.038 (4) | −0.001 (3) | −0.008 (3) | −0.009 (3) |
C29 | 0.051 (5) | 0.064 (5) | 0.070 (6) | 0.000 (4) | 0.005 (4) | 0.010 (5) |
C30 | 0.052 (5) | 0.071 (6) | 0.089 (7) | −0.014 (5) | 0.022 (5) | 0.005 (5) |
C31 | 0.092 (7) | 0.058 (6) | 0.055 (6) | −0.026 (5) | 0.020 (5) | −0.005 (5) |
C32 | 0.102 (8) | 0.043 (5) | 0.062 (6) | −0.014 (5) | −0.010 (5) | −0.004 (4) |
C33 | 0.056 (5) | 0.043 (4) | 0.050 (5) | −0.004 (4) | −0.007 (4) | 0.004 (4) |
C34 | 0.073 (9) | 0.105 (11) | 0.088 (11) | −0.001 (9) | 0.0000 | 0.0000 |
C35 | 0.079 (8) | 0.086 (7) | 0.105 (9) | 0.005 (6) | 0.013 (7) | 0.011 (7) |
C36 | 0.066 (6) | 0.074 (6) | 0.100 (8) | 0.007 (5) | 0.000 (6) | −0.021 (6) |
C37 | 0.067 (8) | 0.062 (8) | 0.096 (11) | 0.022 (7) | 0.0000 | 0.0000 |
C38 | 0.107 (12) | 0.164 (16) | 0.067 (9) | 0.047 (12) | 0.0000 | 0.0000 |
Mn1—Mn2 | 2.9338 (14) | C17—C18 | 1.388 (10) |
Mn1—P1 | 2.314 (2) | C17—H8 | 0.95 |
Mn1—C1 | 1.778 (8) | C18—C19 | 1.374 (11) |
Mn1—C2 | 1.832 (9) | C18—H9 | 0.95 |
Mn1—C3 | 1.833 (8) | C19—C20 | 1.357 (11) |
Mn1—C4 | 1.817 (8) | C19—H10 | 0.95 |
Mn2—P2 | 2.307 (2) | C20—C21 | 1.382 (10) |
Mn2—C5 | 1.836 (9) | C20—H11 | 0.95 |
Mn2—C6 | 1.812 (8) | C21—H12 | 0.95 |
Mn2—C7 | 1.827 (7) | C22—C23 | 1.385 (9) |
Mn2—C8 | 1.782 (9) | C22—C27 | 1.409 (9) |
P1—C9 | 1.843 (7) | C23—C24 | 1.376 (10) |
P1—C10 | 1.821 (6) | C23—H13 | 0.95 |
P1—C28 | 1.839 (7) | C24—C25 | 1.365 (12) |
P2—C9 | 1.820 (7) | C24—H14 | 0.95 |
P2—C16 | 1.837 (7) | C25—C26 | 1.338 (13) |
P2—C22 | 1.824 (7) | C25—H15 | 0.95 |
O1—C1 | 1.160 (8) | C26—C27 | 1.397 (11) |
O2—C2 | 1.154 (9) | C26—H16 | 0.95 |
O3—C3 | 1.142 (8) | C27—H17 | 0.95 |
O4—C4 | 1.147 (8) | C28—C29 | 1.387 (9) |
O5—C5 | 1.153 (8) | C28—C33 | 1.362 (9) |
O6—C6 | 1.136 (8) | C29—C30 | 1.382 (10) |
O7—C7 | 1.149 (8) | C29—H18 | 0.95 |
O8—C8 | 1.144 (9) | C30—C31 | 1.357 (11) |
C9—H1 | 0.95 | C30—H19 | 0.95 |
C9—H2 | 0.95 | C31—C32 | 1.371 (12) |
C10—C11 | 1.378 (9) | C31—H20 | 0.95 |
C10—C15 | 1.393 (9) | C32—C33 | 1.389 (10) |
C11—C12 | 1.388 (11) | C32—H21 | 0.95 |
C11—H3 | 0.95 | C33—H22 | 0.95 |
C12—C13 | 1.360 (13) | C34—C35 | 1.368 (12) |
C12—H4 | 0.95 | C34—C35i | 1.368 (12) |
C13—C14 | 1.366 (12) | C34—H23 | 0.95 |
C13—H5 | 0.95 | C35—C36 | 1.373 (13) |
C14—C15 | 1.361 (10) | C35—H24 | 0.95 |
C14—H6 | 0.95 | C36—C37 | 1.401 (12) |
C15—H7 | 0.95 | C36—H26 | 0.95 |
C16—C17 | 1.400 (9) | C37—C38 | 1.496 (18) |
C16—C21 | 1.386 (9) | ||
O1···C23ii | 3.484 (9) | O6···O6i | 2.901 (12) |
O1···C12iii | 3.512 (10) | O6···C6i | 3.067 (9) |
O2···O2i | 3.484 (12) | O6···C5i | 3.199 (9) |
O3···C32iv | 3.370 (10) | O6···C26iv | 3.406 (10) |
O3···C30iv | 3.503 (10) | O7···C13v | 3.465 (11) |
O3···C33iv | 3.579 (9) | O8···C25vi | 3.579 (11) |
O3···C27iv | 3.583 (9) | C3···C31iv | 3.484 (11) |
O4···C20iii | 3.508 (10) | C6···C6i | 3.582 (15) |
O4···C21iii | 3.577 (9) | C19···C31vii | 3.484 (12) |
O5···O6i | 3.094 (8) | O(6)···C(6)i | 3.067 (9) |
Mn2—Mn1—P1 | 88.80 (6) | C15—C14—H6 | 119.7 |
Mn2—Mn1—C1 | 174.4 (2) | C10—C15—C14 | 121.4 (7) |
Mn2—Mn1—C2 | 81.9 (3) | C10—C15—H7 | 119.3 |
Mn2—Mn1—C3 | 85.5 (3) | C14—C15—H7 | 119.3 |
Mn2—Mn1—C4 | 90.2 (2) | P2—C16—C17 | 122.4 (5) |
P1—Mn1—C1 | 91.9 (2) | P2—C16—C21 | 120.0 (5) |
P1—Mn1—C2 | 91.4 (2) | C17—C16—C21 | 117.6 (7) |
P1—Mn1—C3 | 173.9 (3) | C16—C17—C18 | 120.7 (7) |
P1—Mn1—C4 | 92.6 (2) | C16—C17—H8 | 119.6 |
C1—Mn1—C2 | 92.5 (3) | C18—C17—H8 | 119.7 |
C1—Mn1—C3 | 93.9 (3) | C17—C18—C19 | 120.5 (8) |
C1—Mn1—C4 | 95.4 (3) | C17—C18—H9 | 119.8 |
C2—Mn1—C3 | 90.0 (3) | C19—C18—H9 | 119.8 |
C2—Mn1—C4 | 171.0 (3) | C18—C19—C20 | 118.9 (8) |
C3—Mn1—C4 | 85.3 (3) | C18—C19—H10 | 120.6 |
Mn1—Mn2—P2 | 87.74 (6) | C20—C19—H10 | 120.6 |
Mn1—Mn2—C5 | 89.5 (2) | C19—C20—C21 | 121.9 (7) |
Mn1—Mn2—C6 | 87.2 (3) | C19—C20—H11 | 119.0 |
Mn1—Mn2—C7 | 80.8 (2) | C21—C20—H11 | 119.0 |
Mn1—Mn2—C8 | 174.8 (2) | C16—C21—C20 | 120.4 (7) |
P2—Mn2—C5 | 89.3 (2) | C16—C21—H12 | 119.8 |
P2—Mn2—C6 | 174.5 (3) | C20—C21—H12 | 119.8 |
P2—Mn2—C7 | 93.7 (2) | P2—C22—C23 | 116.6 (5) |
P2—Mn2—C8 | 92.6 (3) | P2—C22—C27 | 123.7 (5) |
C5—Mn2—C6 | 88.5 (3) | C23—C22—C27 | 119.6 (7) |
C5—Mn2—C7 | 169.8 (3) | C22—C23—C24 | 120.1 (7) |
C5—Mn2—C8 | 95.7 (3) | C22—C23—H13 | 120.0 |
C6—Mn2—C7 | 87.5 (3) | C24—C23—H13 | 119.9 |
C6—Mn2—C8 | 92.7 (4) | C23—C24—C25 | 120.7 (8) |
C7—Mn2—C8 | 93.9 (3) | C23—C24—H14 | 119.7 |
Mn1—P1—C9 | 116.1 (2) | C25—C24—H14 | 119.7 |
Mn1—P1—C10 | 113.9 (2) | C24—C25—C26 | 119.7 (8) |
Mn1—P1—C28 | 118.3 (2) | C24—C25—H15 | 120.2 |
C9—P1—C10 | 104.8 (3) | C26—C25—H15 | 120.2 |
C9—P1—C28 | 100.9 (3) | C25—C26—C27 | 122.9 (8) |
C10—P1—C28 | 100.6 (3) | C25—C26—H16 | 118.6 |
Mn2—P2—C9 | 113.1 (2) | C27—C26—H16 | 118.6 |
Mn2—P2—C16 | 117.1 (2) | C22—C27—C26 | 117.0 (7) |
Mn2—P2—C22 | 116.2 (2) | C22—C27—H17 | 121.5 |
C9—P2—C16 | 99.6 (3) | C26—C27—H17 | 121.5 |
C9—P2—C22 | 107.2 (3) | P1—C28—C29 | 121.5 (6) |
C16—P2—C22 | 101.8 (3) | P1—C28—C33 | 119.9 (5) |
Mn1—C1—O1 | 177.6 (7) | C29—C28—C33 | 118.6 (7) |
Mn1—C2—O2 | 176.0 (7) | C28—C29—C30 | 120.5 (8) |
Mn1—C3—O3 | 177.4 (7) | C28—C29—H18 | 119.8 |
Mn1—C4—O4 | 171.8 (6) | C30—C29—H18 | 119.8 |
Mn2—C5—O5 | 176.6 (6) | C29—C30—C31 | 120.2 (8) |
Mn2—C6—O6 | 178.6 (9) | C29—C30—H19 | 119.9 |
Mn2—C7—O7 | 174.9 (7) | C31—C30—H19 | 119.9 |
Mn2—C8—O8 | 178.1 (8) | C30—C31—C32 | 120.1 (8) |
P1—C9—P2 | 115.1 (4) | C30—C31—H20 | 120.0 |
P1—C9—H1 | 108.0 | C32—C31—H20 | 120.0 |
P1—C9—H2 | 108.0 | C31—C32—C33 | 119.7 (8) |
P2—C9—H1 | 108.0 | C31—C32—H21 | 120.1 |
P2—C9—H2 | 108.0 | C33—C32—H21 | 120.1 |
H1—C9—H2 | 109.5 | C28—C33—C32 | 120.9 (7) |
P1—C10—C11 | 126.0 (6) | C28—C33—H22 | 119.6 |
P1—C10—C15 | 117.5 (5) | C32—C33—H22 | 119.6 |
C11—C10—C15 | 116.5 (6) | C35—C34—C35i | 114.6 (14) |
C10—C11—C12 | 122.3 (8) | C35—C34—H23 | 122.7 |
C10—C11—H3 | 118.8 | C35i—C34—H23 | 122.7 |
C12—C11—H3 | 118.8 | C34—C35—C36 | 123.9 (11) |
C11—C12—C13 | 119.0 (8) | C34—C35—H24 | 118.0 |
C11—C12—H4 | 120.5 | C36—C35—H24 | 118.0 |
C13—C12—H4 | 120.5 | C35—C36—C37 | 121.3 (10) |
C12—C13—C14 | 120.2 (8) | C35—C36—H26 | 119.3 |
C12—C13—H5 | 119.9 | C37—C36—H26 | 119.3 |
C14—C13—H5 | 119.9 | C36—C37—C36i | 114.9 (13) |
C13—C14—C15 | 120.6 (8) | C36—C37—C38 | 122.5 (6) |
C13—C14—H6 | 119.7 | C36i—C37—C38 | 122.5 (6) |
Mn1—Mn2—P2—C9 | 41.7 (3) | C4—Mn1—P1—C10 | 172.9 (3) |
Mn1—Mn2—P2—C16 | 156.6 (2) | C4—Mn1—P1—C28 | 55.0 (3) |
Mn1—Mn2—P2—C22 | −82.9 (2) | C5—Mn2—P2—C9 | −47.9 (4) |
Mn1—P1—C9—P2 | −1.2 (5) | C5—Mn2—P2—C16 | 67.0 (3) |
Mn1—P1—C10—C11 | 121.3 (6) | C5—Mn2—P2—C22 | −172.5 (3) |
Mn1—P1—C10—C15 | −58.5 (6) | C7—Mn2—P2—C9 | 122.4 (4) |
Mn1—P1—C28—C29 | −25.8 (7) | C7—Mn2—P2—C16 | −122.7 (3) |
Mn1—P1—C28—C33 | 157.3 (5) | C7—Mn2—P2—C22 | −2.3 (3) |
Mn2—Mn1—P1—C9 | 24.9 (3) | C8—Mn2—P2—C9 | −143.6 (4) |
Mn2—Mn1—P1—C10 | −97.0 (2) | C8—Mn2—P2—C16 | −28.7 (3) |
Mn2—Mn1—P1—C28 | 145.1 (2) | C8—Mn2—P2—C22 | 91.8 (3) |
Mn2—P2—C9—P1 | −33.4 (5) | C9—P1—C10—C11 | −6.6 (7) |
Mn2—P2—C16—C17 | 130.9 (5) | C9—P1—C10—C15 | 173.5 (6) |
Mn2—P2—C16—C21 | −49.6 (7) | C9—P1—C28—C29 | 102.0 (7) |
Mn2—P2—C22—C23 | −52.5 (6) | C9—P1—C28—C33 | −75.0 (6) |
Mn2—P2—C22—C27 | 125.7 (6) | C9—P2—C16—C17 | −106.8 (6) |
P1—Mn1—Mn2—P2 | −33.25 (7) | C9—P2—C16—C21 | 72.6 (6) |
P1—Mn1—Mn2—C5 | 56.1 (2) | C9—P2—C22—C23 | 180.0 (5) |
P1—Mn1—Mn2—C6 | 144.7 (2) | C9—P2—C22—C27 | −1.9 (7) |
P1—Mn1—Mn2—C7 | −127.4 (2) | C10—P1—C28—C29 | −150.5 (6) |
P1—Mn1—Mn2—C8 | −127 (3) | C10—P1—C28—C33 | 32.5 (6) |
P1—C9—P2—C16 | −158.4 (4) | C10—C11—C12—C13 | −1.4 (14) |
P1—C9—P2—C22 | 96.0 (4) | C10—C15—C14—C13 | −1.5 (15) |
P1—C10—C11—C12 | −179.5 (7) | C11—C10—P1—C28 | −111.0 (7) |
P1—C10—C15—C14 | −179.0 (7) | C11—C10—C15—C14 | 1.1 (12) |
P1—C28—C29—C30 | −175.9 (6) | C11—C12—C13—C14 | 1.1 (16) |
P1—C28—C33—C32 | 177.2 (6) | C12—C11—C10—C15 | 0.3 (12) |
P2—Mn2—Mn1—C1 | −131 (2) | C12—C13—C14—C15 | 0.3 (16) |
P2—Mn2—Mn1—C2 | −124.8 (2) | C15—C10—P1—C28 | 69.2 (6) |
P2—Mn2—Mn1—C3 | 144.6 (2) | C16—P2—C22—C23 | 75.9 (6) |
P2—Mn2—Mn1—C4 | 59.3 (2) | C16—P2—C22—C27 | −105.9 (6) |
P2—C9—P1—C10 | 125.4 (4) | C16—C17—C18—C19 | 1.2 (13) |
P2—C9—P1—C28 | −130.4 (4) | C16—C21—C20—C19 | −1.2 (13) |
P2—C16—C17—C18 | 177.8 (6) | C17—C16—P2—C22 | 3.1 (6) |
P2—C16—C21—C20 | −177.9 (6) | C17—C16—C21—C20 | 1.6 (11) |
P2—C22—C23—C24 | −179.7 (6) | C17—C18—C19—C20 | −0.7 (14) |
P2—C22—C27—C26 | −179.3 (6) | C18—C17—C16—C21 | −1.7 (11) |
C1—Mn1—P1—C9 | −160.6 (3) | C18—C19—C20—C21 | 0.7 (13) |
C1—Mn1—P1—C10 | 77.5 (3) | C21—C16—P2—C22 | −177.4 (6) |
C1—Mn1—P1—C28 | −40.4 (3) | C22—C23—C24—C25 | −1.5 (13) |
C2—Mn1—Mn2—C5 | −35.5 (3) | C22—C27—C26—C25 | −0.3 (14) |
C2—Mn1—Mn2—C6 | 53.1 (3) | C23—C22—C27—C26 | −1.2 (11) |
C2—Mn1—Mn2—C7 | 141.0 (3) | C23—C24—C25—C26 | 0.0 (15) |
C2—Mn1—Mn2—C8 | 141 (3) | C24—C23—C22—C27 | 2.0 (11) |
C2—Mn1—P1—C9 | 106.8 (4) | C24—C25—C26—C27 | 0.9 (16) |
C2—Mn1—P1—C10 | −15.1 (3) | C28—C29—C30—C31 | −0.3 (14) |
C2—Mn1—P1—C28 | −133.0 (3) | C28—C33—C32—C31 | −2.1 (12) |
C3—Mn1—Mn2—C5 | −126.1 (3) | C29—C28—C33—C32 | 0.1 (11) |
C3—Mn1—Mn2—C6 | −37.5 (3) | C29—C30—C31—C32 | −1.7 (14) |
C3—Mn1—Mn2—C7 | 50.4 (3) | C30—C29—C28—C33 | 1.1 (12) |
C3—Mn1—Mn2—C8 | 51 (3) | C30—C31—C32—C33 | 2.9 (13) |
C4—Mn1—Mn2—C5 | 148.7 (3) | C34—C35—C36—C37 | −0.5 (14) |
C4—Mn1—Mn2—C6 | −122.8 (3) | C34—C35i—C36i—C37 | −0.5 (14) |
C4—Mn1—Mn2—C7 | −34.8 (3) | C35—C34—C35i—C36i | 0.3 (7) |
C4—Mn1—Mn2—C8 | −35 (3) | C35—C36—C37—C36i | 0.2 (7) |
C4—Mn1—P1—C9 | −65.2 (4) | C35—C36—C37—C38 | −179.8 (7) |
Symmetry codes: (i) −x+1, −y+1, z; (ii) −y+3/2, x, z−1/4; (iii) x+1/2, −y+3/2, z; (iv) −x+3/2, y−1/2, z; (v) −y+3/2, −x+1, z+1/4; (vi) x−1/2, −y+3/2, z; (vii) y−1/2, x, z+1/4. |
Experimental details
(I) | (II) | |
Crystal data | ||
Chemical formula | [Mn2(CO)8(C25H22P2)] | [Mn2(CO)8(C25H22P2)]·0.5C7H8 |
Mr | 718.36 | 764.43 |
Crystal system, space group | Triclinic, P1 | Tetragonal, I41cd |
Temperature (K) | 296 | 294 |
a, b, c (Å) | 12.6428 (13), 15.351 (4), 17.868 (8) | 18.286 (2), 18.286 (2), 41.345 (6) |
α, β, γ (°) | 111.91 (3), 94.05 (3), 90.48 (2) | 90, 90, 90 |
V (Å3) | 3207 (2) | 13824 (3) |
Z | 4 | 16 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 0.94 | 0.87 |
Crystal size (mm) | 0.40 × 0.20 × 0.05 | 0.36 × 0.32 × 0.29 |
Data collection | ||
Diffractometer | Enraf-Nonius CAD-4 diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | Analytical (de Meulenaer & Tompa, 1965) | ψ-scan (North et al., 1968) |
Tmin, Tmax | 0.763, 0.958 | 0.72, 0.77 |
No. of measured, independent and observed reflections | 11815, 11243, 8260 [I > σ(I)] | 3084, 3084, 2520 [I > 1σ(I)] |
Rint | 0.021 | 0.000 |
(sin θ/λ)max (Å−1) | 0.595 | 0.595 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.044, 1.40 | 0.045, 0.038, 1.32 |
No. of reflections | 11243 | 3084 |
No. of parameters | 811 | 438 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.47, −0.46 | 0.48, −0.48 |
Computer programs: CAD-4-PC Software (Enraf-Nonius, 1993), CAD-4-PC Software, TEXSAN (Molecular Structure Corporation, 1997), TEXSAN.
Mn1—Mn2 | 2.9746 (7) | Mn3—Mn4 | 2.9714 (7) |
Mn1—P1 | 2.3033 (9) | Mn3—P3 | 2.3039 (9) |
Mn1—C1 | 1.788 (4) | Mn3—C9 | 1.784 (4) |
Mn1—C2 | 1.832 (4) | Mn3—C10 | 1.815 (4) |
Mn1—C3 | 1.844 (4) | Mn3—C11 | 1.844 (4) |
Mn1—C4 | 1.840 (4) | Mn3—C12 | 1.836 (4) |
Mn2—P2 | 2.3020 (9) | Mn4—P4 | 2.3028 (9) |
Mn2—C5 | 1.788 (4) | Mn4—C13 | 1.781 (4) |
Mn2—C6 | 1.814 (4) | Mn4—C14 | 1.820 (4) |
Mn2—C7 | 1.842 (4) | Mn4—C15 | 1.854 (4) |
Mn2—C8 | 1.827 (4) | Mn4—C16 | 1.827 (4) |
Mn2—Mn1—P1 | 92.17 (3) | Mn4—Mn3—P3 | 91.58 (3) |
Mn2—Mn1—C1 | 175.32 (11) | Mn4—Mn3—C9 | 173.93 (12) |
Mn2—Mn1—C2 | 84.37 (11) | Mn4—Mn3—C10 | 83.89 (13) |
Mn2—Mn1—C3 | 88.25 (10) | Mn4—Mn3—C11 | 90.51 (11) |
Mn2—Mn1—C4 | 84.58 (10) | Mn4—Mn3—C12 | 83.80 (12) |
P1—Mn1—C1 | 91.25 (12) | P3—Mn3—C9 | 92.57 (12) |
P1—Mn1—C2 | 176.48 (11) | P3—Mn3—C10 | 175.30 (13) |
P1—Mn1—C3 | 91.39 (11) | P3—Mn3—C11 | 91.51 (11) |
P1—Mn1—C4 | 90.70 (11) | P3—Mn3—C12 | 90.80 (11) |
C1—Mn1—C2 | 92.24 (16) | C9—Mn3—C10 | 92.04 (17) |
C1—Mn1—C3 | 94.87 (14) | C9—Mn3—C11 | 93.81 (16) |
C1—Mn1—C4 | 92.18 (15) | C9—Mn3—C12 | 91.71 (17) |
C2—Mn1—C3 | 87.89 (16) | C10—Mn3—C11 | 87.27 (17) |
C2—Mn1—C4 | 89.60 (16) | C10—Mn3—C12 | 89.98 (17) |
C3—Mn1—C4 | 172.60 (15) | C11—Mn3—C12 | 173.92 (16) |
Mn1—Mn2—P2 | 86.17 (3) | Mn3—Mn4—P4 | 86.09 (3) |
Mn1—Mn2—C5 | 176.71 (11) | Mn3—Mn4—C13 | 175.71 (11) |
Mn1—Mn2—C6 | 90.71 (12) | Mn3—Mn4—C14 | 91.53 (12) |
Mn1—Mn2—C7 | 82.06 (10) | Mn3—Mn4—C15 | 81.11 (11) |
Mn1—Mn2—C8 | 86.63 (10) | Mn3—Mn4—C16 | 87.43 (10) |
P2—Mn2—C5 | 91.40 (11) | P4—Mn4—C13 | 90.75 (11) |
P2—Mn2—C6 | 176.38 (12) | P4—Mn4—C14 | 176.67 (12) |
P2—Mn2—C7 | 93.32 (11) | P4—Mn4—C15 | 93.21 (10) |
P2—Mn2—C8 | 90.46 (10) | P4—Mn4—C16 | 90.28 (10) |
C5—Mn2—C6 | 91.79 (16) | C13—Mn4—C14 | 91.75 (16) |
C5—Mn2—C7 | 95.89 (14) | C13—Mn4—C15 | 96.19 (15) |
C5—Mn2—C8 | 95.61 (14) | C13—Mn4—C16 | 95.49 (15) |
C6—Mn2—C7 | 88.07 (16) | C14—Mn4—C15 | 88.71 (15) |
C6—Mn2—C8 | 87.52 (16) | C14—Mn4—C16 | 87.29 (15) |
C7—Mn2—C8 | 167.80 (14) | C15—Mn4—C16 | 167.76 (15) |
P1—Mn1—Mn2—P2 | 26.93 (3) | P3—Mn3—Mn4—P4 | −28.44 (3) |
Mn1—Mn2 | 2.9338 (14) | Mn2—P2 | 2.307 (2) |
Mn1—P1 | 2.314 (2) | Mn2—C5 | 1.836 (9) |
Mn1—C1 | 1.778 (8) | Mn2—C6 | 1.812 (8) |
Mn1—C2 | 1.832 (9) | Mn2—C7 | 1.827 (7) |
Mn1—C3 | 1.833 (8) | Mn2—C8 | 1.782 (9) |
Mn1—C4 | 1.817 (8) | ||
Mn2—Mn1—P1 | 88.80 (6) | Mn1—Mn2—P2 | 87.74 (6) |
Mn2—Mn1—C1 | 174.4 (2) | Mn1—Mn2—C5 | 89.5 (2) |
Mn2—Mn1—C2 | 81.9 (3) | Mn1—Mn2—C6 | 87.2 (3) |
Mn2—Mn1—C3 | 85.5 (3) | Mn1—Mn2—C7 | 80.8 (2) |
Mn2—Mn1—C4 | 90.2 (2) | Mn1—Mn2—C8 | 174.8 (2) |
P1—Mn1—C1 | 91.9 (2) | P2—Mn2—C5 | 89.3 (2) |
P1—Mn1—C2 | 91.4 (2) | P2—Mn2—C6 | 174.5 (3) |
P1—Mn1—C3 | 173.9 (3) | P2—Mn2—C7 | 93.7 (2) |
P1—Mn1—C4 | 92.6 (2) | P2—Mn2—C8 | 92.6 (3) |
C1—Mn1—C2 | 92.5 (3) | C5—Mn2—C6 | 88.5 (3) |
C1—Mn1—C3 | 93.9 (3) | C5—Mn2—C7 | 169.8 (3) |
C1—Mn1—C4 | 95.4 (3) | C5—Mn2—C8 | 95.7 (3) |
C2—Mn1—C3 | 90.0 (3) | C6—Mn2—C7 | 87.5 (3) |
C2—Mn1—C4 | 171.0 (3) | C6—Mn2—C8 | 92.7 (4) |
C3—Mn1—C4 | 85.3 (3) | C7—Mn2—C8 | 93.9 (3) |
P1—Mn1—Mn2—P2 | −33.25 (7) |
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The argument is often made that changing the `bite distance' of a bridging ligand in a binuclear compound will change the metal-metal distance. For example, the Rh—Rh bond lengths in [Rh2(µ-L—L)2(CO)2(µ-2,5-dimethylpyrazolatate)]PF6 are 3.060 (3) and 3.220 (2) Å for L—L = dppm and dpam, respectively [dppm is 1,2-bis(diphenylphosphino)methane and dpam is 1,2-bis(diphenylarsino)methane; Janke et al., 1986]. The difference in the bond lengths was proposed to be largely attributable to the difference in the L—L bite distances. The bite distance is certainly important, but the L—M—M—L dihedral angle is an often overlooked parameter that can affect the metal-metal distance.
The crystal structures here reported for Mn2(CO)8(dppm), (I), and Mn2(CO)8(dppm).0.5(toluene), (II), illustrate this point. The increase in the P—Mn—Mn—P dihedral angle from (I) to (II) (see Abstract, and Tables 1 and 2) is accompanied by a shortening of the Mn—Mn bond, but the P···P bite distance is almost unchanged. Simple mechanical considerations require that an increase in the dihedral angle for a given bite distance must be accompanied by a decrease in the Mn—Mn bond length. There are no other significant differences in bond lengths, or in the Mn—Mn—P, Mn—P—C, and P—C—P bond angles. Equivalently, Mn2(CO)8(dpam) has essentially the same Mn—Mn bond length [2.962 (3) Å)] as (I), but the significantly greater bite distance of dpam [3.242 (2) Å] leads to a greater dihedral angle [30.5 (8)°; Hoskins & Steen, 1983]. \sch
The origin of the structural differences between (I) and (II) is not evident. The energy surface for the molecule is apparently very flat with respect to bond distance and dihedral angle, and crystal-packing forces are presumably important in determining the details of the molecular structure. The differences cannot be directly attributed to the presence of toluene solvate molecules in (II), as there are no significantly short complex···complex or complex···solvent contacts in either compound.