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The Mn—Mn bonds in the two independent mol­ecules of the unsolvated title compound, [Mn2(C25H22P2)(CO)8], (I), are 2.9714 (7) and 2.9746 (7) Å. This bond is distinctly shortened in the toluene hemisolvate, [Mn2­(C25­H22P2)(CO)8]·­0.5C7H8, (II), to 2.9338 (14) Å and this shortening is accompanied by an increase in magnitude of the P—Mn—Mn—P torsion angle [26.93 (3) and 28.44 (3)° in (I), and 33.25 (7)° in (II)], while the P...P `bite' is much less affected [3.092 (2) and 3.099 (2) Å in (I), and 3.091 (3) Å in (II)]. The toluene solvate mol­ecule in (II) lies on a twofold axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101013130/fr1342sup1.cif
Contains datablocks common, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101013130/fr1342Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101013130/fr1342IIsup3.hkl
Contains datablock II

CCDC references: 175076; 175077

Comment top

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-LL)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.

Related literature top

For related literature, see: Altomare et al. (1994); Colton & Commons (1975); Hoskins & Steen (1983); Janke et al. (1986).

Experimental top

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.

Refinement top

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].

Computing details top

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.

Figures top
[Figure 1] Fig. 1. The two independent molecules in the unsolvated compound, (I), with 30% probability displacement ellipsoids and the atom-numbering scheme. H atoms are drawn as small spheres of arbitrary radii.
[Figure 2] Fig. 2. The [Mn2(CO)8(dppm)] molecule in the toluene hemisolvate, (II), with 30% probability displacement ellipsoids and the atom-numbering scheme. H atoms are drawn as small spheres of arbitrary radii.
(I) µ-Bis(diphenylphosphino)methane-P:P'-octacarbonyldimanganese(Mn—Mn) top
Crystal data top
[Mn2(CO)8(C25H22P2)]Z = 4
Mr = 718.36F(000) = 1456.00
Triclinic, P1Dx = 1.493 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.6428 (13) ÅCell parameters from 25 reflections
b = 15.351 (4) Åθ = 12.6–13.9°
c = 17.868 (8) ŵ = 0.94 mm1
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
Data collection top
Enraf-Nonius CAD-4
diffractometer
8260 reflections with I > σ(I)
Radiation source: sealed X-ray tubeRint = 0.021
Graphite monochromatorθmax = 25.0°, θmin = 1.5°
ω/2θ scansh = 015
Absorption correction: analytical
(de Meulenaer & Tompa, 1965)
k = 1818
Tmin = 0.763, Tmax = 0.958l = 2121
11815 measured reflections3 standard reflections every 60 min
11243 independent reflections intensity decay: 4.5%
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-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 = 1.40Δρmax = 0.47 e Å3
11243 reflectionsΔρmin = 0.46 e Å3
811 parameters
Crystal data top
[Mn2(CO)8(C25H22P2)]γ = 90.48 (2)°
Mr = 718.36V = 3207 (2) Å3
Triclinic, P1Z = 4
a = 12.6428 (13) ÅMo Kα radiation
b = 15.351 (4) ŵ = 0.94 mm1
c = 17.868 (8) ÅT = 296 K
α = 111.91 (3)°0.40 × 0.20 × 0.05 mm
β = 94.05 (3)°
Data collection top
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 = 0.9583 standard reflections every 60 min
11815 measured reflections intensity decay: 4.5%
11243 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0410 restraints
wR(F2) = 0.044H-atom parameters constrained
S = 1.40Δρmax = 0.47 e Å3
11243 reflectionsΔρmin = 0.46 e Å3
811 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.63360 (4)0.57371 (3)0.80651 (3)0.04516 (14)
Mn20.44401 (4)0.65114 (3)0.74851 (3)0.04396 (14)
Mn30.08395 (4)0.06356 (3)0.80698 (3)0.04845 (15)
Mn40.09363 (4)0.14851 (3)0.75367 (3)0.04508 (14)
P10.57609 (6)0.42131 (6)0.73063 (5)0.0400 (2)
P20.35764 (6)0.51136 (6)0.73066 (5)0.0400 (2)
P30.04169 (6)0.08571 (6)0.72499 (5)0.0403 (2)
P40.17740 (6)0.00971 (6)0.73295 (5)0.0413 (2)
O10.8332 (2)0.5116 (2)0.86144 (17)0.0808 (10)
O20.6966 (2)0.7728 (2)0.90398 (19)0.0961 (11)
O30.5216 (2)0.57678 (19)0.94876 (15)0.0709 (9)
O40.7370 (2)0.5905 (2)0.66782 (17)0.0805 (10)
O50.2512 (2)0.72442 (18)0.69519 (15)0.0703 (9)
O60.5637 (3)0.8247 (2)0.76701 (19)0.0966 (12)
O70.4136 (2)0.74067 (18)0.92422 (15)0.0736 (9)
O80.5188 (2)0.57306 (19)0.58306 (15)0.0709 (9)
O90.2759 (2)0.0019 (2)0.85668 (19)0.0961 (12)
O100.1215 (3)0.2597 (2)0.9120 (2)0.1146 (12)
O110.0505 (2)0.0583 (2)0.94934 (16)0.0793 (10)
O120.2142 (2)0.0886 (2)0.67140 (18)0.0861 (11)
O130.2786 (2)0.22626 (18)0.70636 (16)0.0738 (9)
O140.0223 (3)0.3214 (2)0.77422 (19)0.1001 (12)
O150.1545 (2)0.23252 (18)0.93124 (16)0.0758 (9)
O160.0099 (2)0.07432 (19)0.58648 (15)0.0708 (9)
C10.7539 (3)0.5345 (3)0.8402 (2)0.0561 (11)
C20.6713 (3)0.6973 (3)0.8654 (2)0.0639 (12)
C30.5602 (3)0.5741 (2)0.8922 (2)0.0535 (11)
C40.6935 (3)0.5831 (2)0.7188 (2)0.0542 (11)
C50.3255 (3)0.6950 (2)0.71693 (19)0.0499 (10)
C60.5198 (3)0.7573 (3)0.7612 (2)0.0627 (12)
C70.4255 (3)0.7022 (2)0.8576 (2)0.0516 (10)
C80.4917 (3)0.5992 (2)0.6477 (2)0.0498 (10)
C90.1992 (3)0.0217 (3)0.8372 (2)0.0641 (12)
C100.1065 (3)0.1844 (3)0.8704 (3)0.0733 (13)
C110.0030 (3)0.0579 (2)0.8923 (2)0.0579 (11)
C120.1605 (3)0.0788 (3)0.7218 (2)0.0597 (12)
C130.2067 (3)0.1959 (2)0.7259 (2)0.0520 (10)
C140.0204 (3)0.2542 (3)0.7672 (2)0.0637 (12)
C150.1316 (3)0.1960 (2)0.8640 (2)0.0555 (11)
C160.0282 (3)0.0987 (2)0.6515 (2)0.0515 (11)
C170.4378 (2)0.4082 (2)0.68657 (17)0.0420 (9)
C180.5793 (2)0.3338 (2)0.7781 (2)0.0461 (10)
C190.5451 (3)0.2422 (3)0.7325 (2)0.0614 (12)
C200.5455 (3)0.1747 (3)0.7671 (3)0.0775 (15)
C210.5802 (3)0.1988 (4)0.8464 (3)0.0836 (18)
C220.6154 (3)0.2882 (4)0.8920 (3)0.0772 (16)
C230.6156 (3)0.3565 (3)0.8585 (2)0.0579 (11)
C240.6514 (2)0.3614 (2)0.64272 (18)0.0451 (9)
C250.7421 (3)0.3159 (3)0.6536 (2)0.0603 (12)
C260.8032 (3)0.2729 (3)0.5895 (3)0.0733 (14)
C270.7760 (4)0.2763 (3)0.5158 (3)0.0766 (14)
C280.6879 (4)0.3210 (3)0.5041 (2)0.0798 (15)
C290.6261 (3)0.3641 (3)0.5676 (2)0.0646 (12)
C300.3036 (2)0.5020 (2)0.81872 (18)0.0461 (9)
C310.3279 (3)0.4316 (3)0.8475 (2)0.0576 (11)
C320.2781 (3)0.4269 (4)0.9125 (3)0.0814 (16)
C330.2046 (4)0.4911 (5)0.9482 (3)0.0942 (18)
C340.1807 (3)0.5610 (4)0.9212 (3)0.0876 (16)
C350.2305 (3)0.5672 (3)0.8573 (2)0.0630 (12)
C360.2413 (2)0.4741 (2)0.65634 (18)0.0446 (9)
C370.1527 (3)0.4305 (3)0.6687 (2)0.0598 (11)
C380.0677 (3)0.4019 (3)0.6108 (3)0.0770 (14)
C390.0711 (3)0.4141 (3)0.5396 (3)0.0762 (14)
C400.1593 (3)0.4558 (3)0.5251 (2)0.0774 (14)
C410.2443 (3)0.4863 (3)0.5832 (2)0.0633 (12)
C420.0885 (2)0.0935 (2)0.68320 (17)0.0420 (9)
C430.0368 (2)0.1802 (2)0.76440 (19)0.0454 (9)
C440.0581 (3)0.1674 (3)0.8425 (2)0.0614 (12)
C450.0510 (3)0.2423 (3)0.8682 (3)0.0772 (15)
C460.0227 (3)0.3276 (3)0.8177 (3)0.0796 (16)
C470.0022 (3)0.3421 (3)0.7403 (3)0.0742 (14)
C480.0095 (3)0.2690 (2)0.7131 (2)0.0574 (11)
C490.1348 (2)0.1410 (2)0.63565 (19)0.0456 (9)
C500.2265 (3)0.1839 (3)0.6448 (2)0.0637 (12)
C510.3025 (3)0.2236 (3)0.5811 (3)0.0776 (14)
C520.2884 (4)0.2196 (3)0.5078 (3)0.0783 (14)
C530.1988 (4)0.1769 (3)0.4977 (2)0.0802 (15)
C540.1213 (3)0.1375 (3)0.5608 (2)0.0650 (12)
C550.2442 (2)0.0030 (2)0.82202 (18)0.0472 (10)
C560.3229 (3)0.0649 (3)0.8657 (2)0.0617 (12)
C570.3755 (3)0.0608 (3)0.9344 (3)0.0799 (14)
C580.3504 (4)0.0104 (4)0.9597 (3)0.0872 (17)
C590.2736 (3)0.0773 (3)0.9182 (3)0.0786 (16)
C600.2212 (3)0.0751 (3)0.8473 (2)0.0596 (12)
C610.2811 (2)0.0215 (2)0.66161 (19)0.0464 (10)
C620.2641 (3)0.0103 (3)0.5880 (2)0.0650 (12)
C630.3388 (4)0.0358 (3)0.5316 (2)0.0780 (15)
C640.4313 (4)0.0729 (3)0.5481 (3)0.0834 (16)
C650.4504 (3)0.0839 (3)0.6200 (3)0.0813 (15)
C660.3754 (3)0.0592 (3)0.6767 (2)0.0630 (12)
H10.43890.39530.63030.050*
H20.40470.35650.69400.050*
H30.52120.22530.67710.074*
H40.52170.11190.73550.093*
H50.57970.15280.87020.100*
H60.64010.30400.94710.093*
H70.64050.41880.89060.070*
H80.76230.31430.70520.072*
H90.86450.24090.59710.088*
H100.81890.24730.47220.092*
H110.66870.32260.45230.096*
H120.56520.39610.55920.078*
H130.37860.38670.82270.069*
H140.29500.37890.93230.098*
H150.16990.48670.99220.113*
H160.12980.60550.94640.105*
H170.21450.61690.83940.076*
H180.14970.41980.71760.072*
H190.00620.37340.62100.092*
H200.01260.39380.50000.091*
H210.16220.46390.47510.093*
H220.30500.51570.57290.076*
H230.12250.14640.68790.050*
H240.07700.10250.62770.050*
H250.07760.10760.87850.074*
H260.06620.23340.92180.093*
H270.01710.37790.83640.095*
H280.01700.40240.70510.089*
H290.00420.27950.65890.069*
H300.23770.18640.69600.076*
H310.36460.25360.58850.093*
H320.34070.24640.46400.094*
H330.18910.17410.44640.096*
H340.05910.10820.55260.078*
H350.34010.11410.84810.074*
H360.42900.10700.96410.096*
H370.38710.01311.00700.105*
H380.25580.12510.93730.094*
H390.17000.12320.81670.071*
H400.19990.01540.57630.078*
H410.32600.02760.48170.094*
H420.48260.09110.50930.100*
H430.51540.10870.63140.098*
H440.38900.06820.72620.076*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0455 (3)0.0485 (3)0.0396 (3)0.0002 (2)0.0017 (2)0.0153 (2)
Mn20.0493 (3)0.0428 (3)0.0413 (3)0.0022 (2)0.0013 (2)0.0179 (2)
Mn30.0525 (3)0.0465 (3)0.0431 (3)0.0072 (2)0.0147 (2)0.0110 (2)
Mn40.0518 (3)0.0411 (3)0.0435 (3)0.0050 (2)0.0059 (2)0.0166 (2)
P10.0417 (4)0.0449 (5)0.0351 (4)0.0037 (4)0.0024 (3)0.0171 (4)
P20.0414 (4)0.0427 (5)0.0366 (4)0.0027 (4)0.0001 (3)0.0160 (4)
P30.0454 (5)0.0415 (5)0.0346 (4)0.0029 (4)0.0083 (3)0.0142 (4)
P40.0444 (4)0.0424 (5)0.0392 (5)0.0038 (4)0.0077 (4)0.0169 (4)
O10.0521 (16)0.118 (2)0.094 (2)0.0061 (15)0.0038 (14)0.0663 (19)
O20.090 (2)0.0612 (19)0.103 (2)0.0116 (16)0.0142 (17)0.0046 (17)
O30.0735 (17)0.098 (2)0.0443 (15)0.0142 (14)0.0128 (13)0.0283 (15)
O40.0777 (19)0.106 (2)0.0714 (19)0.0118 (16)0.0138 (15)0.0479 (17)
O50.0696 (17)0.0767 (18)0.0698 (18)0.0266 (14)0.0060 (13)0.0330 (15)
O60.112 (2)0.077 (2)0.108 (3)0.0340 (18)0.0061 (19)0.0458 (19)
O70.102 (2)0.0667 (17)0.0443 (15)0.0144 (15)0.0044 (14)0.0122 (13)
O80.0802 (18)0.0849 (19)0.0475 (16)0.0113 (14)0.0109 (13)0.0236 (14)
O90.080 (2)0.104 (2)0.109 (3)0.0028 (17)0.0463 (18)0.039 (2)
O100.113 (3)0.066 (2)0.123 (3)0.0225 (18)0.037 (2)0.0175 (19)
O110.097 (2)0.090 (2)0.0460 (16)0.0009 (16)0.0008 (15)0.0215 (15)
O120.080 (2)0.103 (2)0.085 (2)0.0263 (17)0.0028 (16)0.0472 (19)
O130.0745 (18)0.0730 (18)0.0761 (19)0.0204 (14)0.0061 (14)0.0308 (15)
O140.124 (3)0.075 (2)0.105 (3)0.0461 (19)0.0145 (19)0.0359 (18)
O150.104 (2)0.0704 (18)0.0448 (16)0.0045 (15)0.0028 (14)0.0130 (14)
O160.0797 (18)0.0833 (19)0.0473 (16)0.0035 (14)0.0026 (13)0.0235 (14)
C10.053 (2)0.072 (3)0.049 (2)0.0061 (18)0.0022 (16)0.0292 (19)
C20.057 (2)0.062 (3)0.058 (2)0.0046 (19)0.0050 (18)0.008 (2)
C30.051 (2)0.060 (2)0.046 (2)0.0063 (16)0.0040 (16)0.0172 (18)
C40.053 (2)0.057 (2)0.053 (2)0.0051 (16)0.0005 (17)0.0218 (18)
C50.062 (2)0.048 (2)0.0402 (19)0.0054 (16)0.0085 (16)0.0155 (16)
C60.072 (3)0.062 (3)0.058 (2)0.002 (2)0.0010 (19)0.027 (2)
C70.063 (2)0.0426 (19)0.048 (2)0.0018 (16)0.0020 (17)0.0164 (17)
C80.0502 (19)0.049 (2)0.053 (2)0.0042 (15)0.0021 (16)0.0221 (17)
C90.069 (3)0.064 (2)0.059 (2)0.0087 (19)0.0226 (19)0.0181 (19)
C100.067 (3)0.065 (3)0.074 (3)0.010 (2)0.021 (2)0.007 (2)
C110.066 (2)0.056 (2)0.045 (2)0.0001 (17)0.0172 (18)0.0087 (18)
C120.063 (2)0.054 (2)0.064 (3)0.0166 (18)0.0173 (19)0.0211 (19)
C130.062 (2)0.0437 (19)0.049 (2)0.0027 (16)0.0021 (17)0.0175 (16)
C140.078 (3)0.057 (2)0.055 (2)0.013 (2)0.0071 (19)0.0195 (19)
C150.064 (2)0.047 (2)0.058 (2)0.0057 (17)0.0119 (18)0.0209 (19)
C160.056 (2)0.046 (2)0.054 (2)0.0072 (16)0.0100 (17)0.0195 (17)
C170.0440 (17)0.0445 (18)0.0348 (17)0.0022 (14)0.0005 (13)0.0123 (14)
C180.0406 (17)0.054 (2)0.053 (2)0.0090 (15)0.0091 (15)0.0302 (17)
C190.062 (2)0.057 (2)0.072 (3)0.0046 (18)0.0053 (19)0.032 (2)
C200.077 (3)0.061 (3)0.107 (4)0.000 (2)0.008 (3)0.045 (3)
C210.071 (3)0.100 (4)0.119 (4)0.016 (3)0.023 (3)0.083 (4)
C220.076 (3)0.105 (4)0.075 (3)0.017 (3)0.012 (2)0.061 (3)
C230.059 (2)0.074 (3)0.054 (2)0.0100 (18)0.0059 (17)0.038 (2)
C240.0463 (18)0.0477 (19)0.0412 (18)0.0040 (15)0.0082 (14)0.0156 (15)
C250.053 (2)0.075 (3)0.059 (2)0.0095 (18)0.0092 (17)0.030 (2)
C260.059 (2)0.083 (3)0.082 (3)0.020 (2)0.024 (2)0.032 (3)
C270.091 (3)0.067 (3)0.072 (3)0.016 (2)0.042 (2)0.019 (2)
C280.117 (4)0.078 (3)0.052 (2)0.028 (3)0.034 (2)0.029 (2)
C290.084 (3)0.066 (3)0.050 (2)0.028 (2)0.0193 (19)0.0255 (19)
C300.0445 (18)0.056 (2)0.0362 (17)0.0061 (15)0.0017 (14)0.0161 (16)
C310.055 (2)0.073 (3)0.051 (2)0.0124 (18)0.0063 (16)0.0311 (19)
C320.073 (3)0.121 (4)0.070 (3)0.025 (3)0.011 (2)0.062 (3)
C330.081 (3)0.156 (5)0.046 (3)0.025 (3)0.005 (2)0.039 (3)
C340.077 (3)0.116 (4)0.053 (3)0.002 (3)0.020 (2)0.009 (3)
C350.066 (2)0.068 (3)0.051 (2)0.0070 (19)0.0127 (18)0.0151 (19)
C360.0440 (18)0.0417 (18)0.0452 (19)0.0064 (14)0.0039 (14)0.0143 (15)
C370.057 (2)0.065 (2)0.057 (2)0.0045 (18)0.0073 (17)0.0245 (19)
C380.057 (2)0.079 (3)0.087 (3)0.016 (2)0.014 (2)0.026 (3)
C390.068 (3)0.079 (3)0.067 (3)0.002 (2)0.024 (2)0.016 (2)
C400.082 (3)0.093 (3)0.053 (2)0.006 (2)0.016 (2)0.027 (2)
C410.059 (2)0.081 (3)0.052 (2)0.0024 (19)0.0086 (17)0.029 (2)
C420.0467 (18)0.0437 (18)0.0365 (17)0.0051 (14)0.0081 (13)0.0152 (14)
C430.0418 (17)0.050 (2)0.048 (2)0.0029 (14)0.0013 (14)0.0238 (16)
C440.071 (2)0.067 (2)0.052 (2)0.0031 (19)0.0072 (18)0.0291 (19)
C450.084 (3)0.093 (3)0.077 (3)0.005 (3)0.005 (2)0.059 (3)
C460.068 (3)0.082 (3)0.119 (4)0.003 (2)0.004 (3)0.073 (3)
C470.071 (3)0.054 (2)0.107 (4)0.0054 (19)0.011 (2)0.040 (3)
C480.063 (2)0.050 (2)0.063 (2)0.0008 (17)0.0095 (18)0.0243 (19)
C490.0493 (19)0.0393 (18)0.0461 (19)0.0046 (14)0.0011 (15)0.0142 (15)
C500.052 (2)0.078 (3)0.059 (2)0.0005 (19)0.0034 (17)0.023 (2)
C510.058 (2)0.081 (3)0.084 (3)0.008 (2)0.011 (2)0.024 (3)
C520.087 (3)0.061 (3)0.072 (3)0.005 (2)0.036 (2)0.015 (2)
C530.114 (4)0.072 (3)0.051 (2)0.011 (3)0.019 (2)0.023 (2)
C540.082 (3)0.064 (2)0.051 (2)0.014 (2)0.0077 (19)0.0272 (19)
C550.0485 (19)0.054 (2)0.0389 (18)0.0120 (15)0.0076 (14)0.0160 (16)
C560.061 (2)0.065 (2)0.053 (2)0.0030 (18)0.0012 (18)0.0162 (19)
C570.068 (3)0.097 (3)0.058 (3)0.007 (2)0.012 (2)0.014 (2)
C580.077 (3)0.135 (5)0.056 (3)0.026 (3)0.001 (2)0.044 (3)
C590.076 (3)0.112 (4)0.070 (3)0.022 (3)0.012 (2)0.059 (3)
C600.061 (2)0.068 (3)0.056 (2)0.0134 (18)0.0082 (17)0.031 (2)
C610.0477 (19)0.0442 (18)0.049 (2)0.0017 (14)0.0145 (15)0.0176 (16)
C620.063 (2)0.080 (3)0.060 (2)0.0113 (19)0.0193 (19)0.034 (2)
C630.089 (3)0.092 (3)0.065 (3)0.011 (3)0.033 (2)0.039 (2)
C640.081 (3)0.082 (3)0.095 (3)0.014 (2)0.050 (3)0.034 (3)
C650.064 (3)0.091 (3)0.095 (3)0.028 (2)0.030 (2)0.038 (3)
C660.060 (2)0.069 (3)0.065 (2)0.0151 (19)0.0197 (19)0.028 (2)
Geometric parameters (Å, º) top
Mn1—Mn22.9746 (7)C28—C291.382 (5)
Mn1—P12.3033 (9)C28—H110.95
Mn1—C11.788 (4)C29—H120.95
Mn1—C21.832 (4)C30—C311.387 (4)
Mn1—C31.844 (4)C30—C351.387 (5)
Mn1—C41.840 (4)C31—C321.383 (5)
Mn2—P22.3020 (9)C31—H130.95
Mn2—C51.788 (4)C32—C331.368 (7)
Mn2—C61.814 (4)C32—H140.95
Mn2—C71.842 (4)C33—C341.359 (7)
Mn2—C81.827 (4)C33—H150.95
Mn3—Mn42.9714 (7)C34—C351.374 (5)
Mn3—P32.3039 (9)C34—H160.95
Mn3—C91.784 (4)C35—H170.95
Mn3—C101.815 (4)C36—C371.373 (4)
Mn3—C111.844 (4)C36—C411.391 (4)
Mn3—C121.836 (4)C37—C381.383 (5)
Mn4—P42.3028 (9)C37—H180.95
Mn4—C131.781 (4)C38—C391.357 (6)
Mn4—C141.820 (4)C38—H190.95
Mn4—C151.854 (4)C39—C401.367 (6)
Mn4—C161.827 (4)C39—H200.95
P1—C171.844 (3)C40—C411.386 (5)
P1—C181.837 (3)C40—H210.95
P1—C241.835 (3)C41—H220.95
P2—C171.834 (3)C42—H230.95
P2—C301.812 (3)C42—H240.95
P2—C361.843 (3)C43—C441.382 (4)
P3—C421.842 (3)C43—C481.392 (4)
P3—C431.833 (3)C44—C451.388 (5)
P3—C491.833 (3)C44—H250.95
P4—C421.828 (3)C45—C461.353 (6)
P4—C551.824 (3)C45—H260.95
P4—C611.834 (3)C46—C471.359 (6)
O1—C11.150 (4)C46—H270.95
O2—C21.135 (4)C47—C481.381 (5)
O3—C31.140 (4)C47—H280.95
O4—C41.136 (4)C48—H290.95
O5—C51.151 (4)C49—C501.378 (5)
O6—C61.137 (4)C49—C541.381 (5)
O7—C71.137 (4)C50—C511.381 (5)
O8—C81.150 (4)C50—H300.95
O9—C91.153 (4)C51—C521.357 (6)
O10—C101.143 (4)C51—H310.95
O11—C111.144 (4)C52—C531.361 (6)
O12—C121.145 (4)C52—H320.95
O13—C131.151 (4)C53—C541.386 (5)
O14—C141.138 (4)C53—H330.95
O15—C151.135 (4)C54—H340.95
O16—C161.147 (4)C55—C561.397 (5)
C17—H10.95C55—C601.379 (5)
C17—H20.95C56—C571.376 (5)
C18—C191.383 (5)C56—H350.95
C18—C231.388 (4)C57—C581.372 (6)
C19—C201.391 (5)C57—H360.95
C19—H30.95C58—C591.363 (6)
C20—C211.362 (6)C58—H370.95
C20—H40.95C59—C601.399 (5)
C21—C221.360 (6)C59—H380.95
C21—H50.95C60—H390.95
C22—C231.387 (5)C61—C621.390 (5)
C22—H60.95C61—C661.382 (4)
C23—H70.95C62—C631.381 (5)
C24—C251.386 (4)C62—H400.95
C24—C291.373 (4)C63—C641.366 (6)
C25—C261.383 (5)C63—H410.95
C25—H80.95C64—C651.362 (6)
C26—C271.358 (5)C64—H420.95
C26—H90.95C65—C661.386 (5)
C27—C281.357 (6)C65—H430.95
C27—H100.95C66—H440.95
O1···O14i3.375 (4)O6···C50ii3.526 (5)
O1···C46ii3.405 (5)O7···C59v3.352 (5)
O1···C33iii3.484 (5)O7···C22iii3.517 (5)
O2···C57iii3.257 (5)O8···O8iv2.980 (5)
O2···C45ii3.292 (5)O8···C29iv3.579 (4)
O2···O15iii3.408 (4)O9···C58vi3.416 (5)
O2···C44ii3.585 (5)O10···C34vii3.353 (5)
O3···C22iii3.428 (5)O10···C22viii3.370 (5)
O3···C32iii3.433 (5)O11···O11vi3.290 (6)
O3···O3iii3.542 (5)O11···C45vi3.425 (6)
O4···C47ii3.458 (5)O11···C44vi3.456 (4)
O4···C40iv3.597 (5)O13···C313.240 (4)
O5···C60v3.305 (4)O13···C193.363 (4)
O5···C48v3.333 (4)O13···C53ix3.506 (5)
O5···C28iv3.508 (4)O13···C173.566 (4)
O5···C42v3.545 (4)O14···C25viii3.533 (5)
O5···C47v3.590 (5)O15···C323.493 (5)
O6···O9ii3.167 (4)O16···O16ix3.111 (5)
Mn2—Mn1—P192.17 (3)C24—C25—H8119.8
Mn2—Mn1—C1175.32 (11)C26—C25—H8119.8
Mn2—Mn1—C284.37 (11)C25—C26—C27120.3 (4)
Mn2—Mn1—C388.25 (10)C25—C26—H9119.9
Mn2—Mn1—C484.58 (10)C27—C26—H9119.9
P1—Mn1—C191.25 (12)C26—C27—C28120.3 (4)
P1—Mn1—C2176.48 (11)C26—C27—H10119.9
P1—Mn1—C391.39 (11)C28—C27—H10119.9
P1—Mn1—C490.70 (11)C27—C28—C29119.9 (4)
C1—Mn1—C292.24 (16)C27—C28—H11120.0
C1—Mn1—C394.87 (14)C29—C28—H11120.0
C1—Mn1—C492.18 (15)C24—C29—C28121.1 (3)
C2—Mn1—C387.89 (16)C24—C29—H12119.5
C2—Mn1—C489.60 (16)C28—C29—H12119.5
C3—Mn1—C4172.60 (15)P2—C30—C31123.9 (3)
Mn1—Mn2—P286.17 (3)P2—C30—C35117.6 (3)
Mn1—Mn2—C5176.71 (11)C31—C30—C35118.5 (3)
Mn1—Mn2—C690.71 (12)C30—C31—C32119.9 (4)
Mn1—Mn2—C782.06 (10)C30—C31—H13120.1
Mn1—Mn2—C886.63 (10)C32—C31—H13120.1
P2—Mn2—C591.40 (11)C31—C32—C33120.3 (4)
P2—Mn2—C6176.38 (12)C31—C32—H14119.9
P2—Mn2—C793.32 (11)C33—C32—H14119.9
P2—Mn2—C890.46 (10)C32—C33—C34120.6 (4)
C5—Mn2—C691.79 (16)C32—C33—H15119.7
C5—Mn2—C795.89 (14)C34—C33—H15119.7
C5—Mn2—C895.61 (14)C33—C34—C35119.8 (4)
C6—Mn2—C788.07 (16)C33—C34—H16120.1
C6—Mn2—C887.52 (16)C35—C34—H16120.1
C7—Mn2—C8167.80 (14)C30—C35—C34121.0 (4)
Mn4—Mn3—P391.58 (3)C30—C35—H17119.5
Mn4—Mn3—C9173.93 (12)C34—C35—H17119.5
Mn4—Mn3—C1083.89 (13)P2—C36—C37122.5 (3)
Mn4—Mn3—C1190.51 (11)P2—C36—C41119.4 (3)
Mn4—Mn3—C1283.80 (12)C37—C36—C41118.1 (3)
P3—Mn3—C992.57 (12)C36—C37—C38120.8 (4)
P3—Mn3—C10175.30 (13)C36—C37—H18119.6
P3—Mn3—C1191.51 (11)C38—C37—H18119.6
P3—Mn3—C1290.80 (11)C37—C38—C39120.7 (4)
C9—Mn3—C1092.04 (17)C37—C38—H19119.6
C9—Mn3—C1193.81 (16)C39—C38—H19119.6
C9—Mn3—C1291.71 (17)C38—C39—C40119.7 (4)
C10—Mn3—C1187.27 (17)C38—C39—H20120.2
C10—Mn3—C1289.98 (17)C40—C39—H20120.2
C11—Mn3—C12173.92 (16)C39—C40—C41120.2 (4)
Mn3—Mn4—P486.09 (3)C39—C40—H21119.9
Mn3—Mn4—C13175.71 (11)C41—C40—H21119.9
Mn3—Mn4—C1491.53 (12)C36—C41—C40120.5 (4)
Mn3—Mn4—C1581.11 (11)C36—C41—H22119.8
Mn3—Mn4—C1687.43 (10)C40—C41—H22119.8
P4—Mn4—C1390.75 (11)P3—C42—P4114.80 (16)
P4—Mn4—C14176.67 (12)P3—C42—H23108.1
P4—Mn4—C1593.21 (10)P3—C42—H24108.1
P4—Mn4—C1690.28 (10)P4—C42—H23108.1
C13—Mn4—C1491.75 (16)P4—C42—H24108.1
C13—Mn4—C1596.19 (15)H23—C42—H24109.5
C13—Mn4—C1695.49 (15)P3—C43—C44123.3 (3)
C14—Mn4—C1588.71 (15)P3—C43—C48118.3 (3)
C14—Mn4—C1687.29 (15)C44—C43—C48118.4 (3)
C15—Mn4—C16167.76 (15)C43—C44—C45119.8 (4)
Mn1—P1—C17114.74 (10)C43—C44—H25120.1
Mn1—P1—C18119.20 (11)C45—C44—H25120.1
Mn1—P1—C24114.87 (10)C44—C45—C46120.7 (4)
C17—P1—C18102.14 (14)C44—C45—H26119.6
C17—P1—C24103.41 (13)C46—C45—H26119.6
C18—P1—C24100.17 (14)C45—C46—C47120.6 (4)
Mn2—P2—C17113.60 (10)C45—C46—H27119.7
Mn2—P2—C30116.91 (11)C47—C46—H27119.7
Mn2—P2—C36117.50 (10)C46—C47—C48119.9 (4)
C17—P2—C30107.07 (15)C46—C47—H28120.1
C17—P2—C3698.35 (13)C48—C47—H28120.1
C30—P2—C36101.11 (14)C43—C48—C47120.6 (4)
Mn3—P3—C42114.73 (10)C43—C48—H29119.7
Mn3—P3—C43120.15 (11)C47—C48—H29119.7
Mn3—P3—C49114.39 (10)P3—C49—C50118.1 (3)
C42—P3—C43101.61 (14)P3—C49—C54123.7 (3)
C42—P3—C49104.03 (14)C50—C49—C54118.0 (3)
C43—P3—C4999.53 (14)C49—C50—C51121.4 (4)
Mn4—P4—C42112.66 (10)C49—C50—H30119.3
Mn4—P4—C55116.57 (11)C51—C50—H30119.3
Mn4—P4—C61117.62 (11)C50—C51—C52120.0 (4)
C42—P4—C55107.26 (15)C50—C51—H31120.0
C42—P4—C6198.58 (14)C52—C51—H31120.0
C55—P4—C61102.10 (14)C51—C52—C53119.4 (4)
Mn1—C1—O1177.7 (3)C51—C52—H32120.3
Mn1—C2—O2177.4 (4)C53—C52—H32120.3
Mn1—C3—O3174.9 (3)C52—C53—C54121.3 (4)
Mn1—C4—O4175.3 (3)C52—C53—H33119.4
Mn2—C5—O5177.8 (3)C54—C53—H33119.4
Mn2—C6—O6176.9 (4)C49—C54—C53119.8 (4)
Mn2—C7—O7174.3 (3)C49—C54—H34120.1
Mn2—C8—O8174.2 (3)C53—C54—H34120.1
Mn3—C9—O9177.0 (4)P4—C55—C56116.9 (3)
Mn3—C10—O10178.2 (4)P4—C55—C60123.6 (3)
Mn3—C11—O11174.2 (3)C56—C55—C60119.5 (3)
Mn3—C12—O12175.4 (3)C55—C56—C57120.2 (4)
Mn4—C13—O13178.5 (3)C55—C56—H35119.9
Mn4—C14—O14177.3 (4)C57—C56—H35119.9
Mn4—C15—O15174.1 (3)C56—C57—C58119.7 (4)
Mn4—C16—O16174.0 (3)C56—C57—H36120.2
P1—C17—P2114.82 (15)C58—C57—H36120.2
P1—C17—H1108.1C57—C58—C59121.1 (4)
P1—C17—H2108.1C57—C58—H37119.4
P2—C17—H1108.1C59—C58—H37119.4
P2—C17—H2108.1C58—C59—C60119.8 (4)
H1—C17—H2109.5C58—C59—H38120.1
P1—C18—C19119.2 (3)C60—C59—H38120.1
P1—C18—C23122.0 (3)C55—C60—C59119.6 (4)
C19—C18—C23118.8 (3)C55—C60—H39120.2
C18—C19—C20120.5 (4)C59—C60—H39120.2
C18—C19—H3119.8P4—C61—C62119.6 (3)
C20—C19—H3119.8P4—C61—C66122.5 (3)
C19—C20—C21119.8 (4)C62—C61—C66117.9 (3)
C19—C20—H4120.1C61—C62—C63121.3 (4)
C21—C20—H4120.1C61—C62—H40119.3
C20—C21—C22120.6 (4)C63—C62—H40119.3
C20—C21—H5119.7C62—C63—C64119.6 (4)
C22—C21—H5119.7C62—C63—H41120.2
C21—C22—C23120.4 (4)C64—C63—H41120.2
C21—C22—H6119.8C63—C64—C65120.3 (4)
C23—C22—H6119.8C63—C64—H42119.8
C18—C23—C22120.0 (4)C65—C64—H42119.8
C18—C23—H7120.0C64—C65—C66120.4 (4)
C22—C23—H7120.0C64—C65—H43119.8
P1—C24—C25118.5 (2)C66—C65—H43119.8
P1—C24—C29123.2 (3)C61—C66—C65120.5 (4)
C25—C24—C29118.1 (3)C61—C66—H44119.8
C24—C25—C26120.3 (3)C65—C66—H44119.8
Mn1—Mn2—P2—C1741.91 (10)C10—Mn3—Mn4—C16119.26 (17)
Mn1—Mn2—P2—C3083.61 (12)C11—Mn3—Mn4—C1320.5 (14)
Mn1—Mn2—P2—C36155.87 (11)C11—Mn3—Mn4—C14119.25 (16)
Mn1—P1—C17—P215.44 (19)C11—Mn3—Mn4—C1530.79 (15)
Mn1—P1—C18—C19179.8 (2)C11—Mn3—Mn4—C16153.54 (15)
Mn1—P1—C18—C230.1 (3)C11—Mn3—P3—C4277.90 (15)
Mn1—P1—C24—C2586.6 (3)C11—Mn3—P3—C4343.70 (16)
Mn1—P1—C24—C2989.2 (3)C11—Mn3—P3—C49161.97 (16)
Mn2—Mn1—P1—C1711.48 (11)C12—Mn3—Mn4—C13161.6 (14)
Mn2—Mn1—P1—C18133.00 (11)C12—Mn3—Mn4—C1458.59 (16)
Mn2—Mn1—P1—C24108.19 (11)C12—Mn3—Mn4—C15147.05 (15)
Mn2—P2—C17—P144.50 (18)C12—Mn3—Mn4—C1628.62 (15)
Mn2—P2—C30—C31124.5 (3)C12—Mn3—P3—C4296.47 (16)
Mn2—P2—C30—C3558.2 (3)C12—Mn3—P3—C43141.93 (16)
Mn2—P2—C36—C37142.2 (3)C12—Mn3—P3—C4923.66 (16)
Mn2—P2—C36—C4140.8 (3)C13—Mn4—P4—C42139.33 (15)
Mn3—Mn4—P4—C4243.57 (10)C13—Mn4—P4—C5596.05 (16)
Mn3—Mn4—P4—C5581.05 (12)C13—Mn4—P4—C6125.70 (16)
Mn3—Mn4—P4—C61157.20 (12)C14—Mn4—P4—C421 (2)
Mn3—P3—C42—P415.34 (19)C14—Mn4—P4—C55125 (2)
Mn3—P3—C43—C440.5 (3)C14—Mn4—P4—C61113 (2)
Mn3—P3—C43—C48179.2 (2)C15—Mn4—P4—C42124.43 (15)
Mn3—P3—C49—C5082.5 (3)C15—Mn4—P4—C550.20 (16)
Mn3—P3—C49—C5493.7 (3)C15—Mn4—P4—C61121.94 (16)
Mn4—Mn3—P3—C4212.65 (11)C16—Mn4—P4—C4243.83 (15)
Mn4—Mn3—P3—C43134.25 (11)C16—Mn4—P4—C55168.46 (16)
Mn4—Mn3—P3—C49107.48 (12)C16—Mn4—P4—C6169.80 (16)
Mn4—P4—C42—P345.73 (18)C17—P1—C18—C1952.6 (3)
Mn4—P4—C55—C5657.8 (3)C17—P1—C18—C23127.8 (3)
Mn4—P4—C55—C60122.4 (3)C17—P1—C24—C25147.6 (3)
Mn4—P4—C61—C6244.1 (3)C17—P1—C24—C2936.5 (3)
Mn4—P4—C61—C66138.2 (3)C17—P2—C30—C314.2 (3)
P1—Mn1—Mn2—P226.93 (3)C17—P2—C30—C35173.1 (3)
P1—Mn1—Mn2—C6151.23 (12)C17—P2—C36—C3795.7 (3)
P1—Mn1—Mn2—C7120.82 (11)C17—P2—C36—C4181.4 (3)
P1—Mn1—Mn2—C863.76 (10)C18—P1—C24—C2542.4 (3)
P1—C17—P2—C3086.10 (18)C18—P1—C24—C29141.7 (3)
P1—C17—P2—C36169.49 (17)C18—C19—C20—C210.2 (6)
P1—C18—C19—C20179.3 (3)C18—C23—C22—C210.2 (6)
P1—C18—C23—C22179.3 (3)C19—C18—P1—C2453.7 (3)
P1—C24—C25—C26177.6 (3)C19—C18—C23—C221.0 (5)
P1—C24—C29—C28177.3 (3)C19—C20—C21—C220.7 (7)
P2—Mn2—Mn1—C2152.44 (13)C20—C19—C18—C231.1 (5)
P2—Mn2—Mn1—C364.40 (11)C20—C21—C22—C230.7 (7)
P2—Mn2—Mn1—C4117.43 (11)C23—C18—P1—C24126.0 (3)
P2—C17—P1—C18115.00 (18)C24—C25—C26—C271.2 (6)
P2—C17—P1—C24141.30 (17)C24—C29—C28—C271.0 (7)
P2—C30—C31—C32176.3 (3)C25—C24—C29—C281.4 (6)
P2—C30—C35—C34175.7 (3)C25—C26—C27—C280.8 (7)
P2—C36—C37—C38178.8 (3)C26—C25—C24—C291.5 (5)
P2—C36—C41—C40177.7 (3)C26—C27—C28—C290.7 (7)
P3—Mn3—Mn4—P428.44 (3)C30—P2—C36—C3713.7 (3)
P3—Mn3—Mn4—C14149.23 (12)C30—P2—C36—C41169.3 (3)
P3—Mn3—Mn4—C15122.31 (11)C30—C31—C32—C330.3 (6)
P3—Mn3—Mn4—C1662.01 (10)C30—C35—C34—C331.2 (6)
P3—C42—P4—C5583.85 (18)C31—C30—P2—C36106.6 (3)
P3—C42—P4—C61170.55 (17)C31—C30—C35—C341.8 (5)
P3—C43—C44—C45179.0 (3)C31—C32—C33—C341.0 (7)
P3—C43—C48—C47178.5 (3)C32—C31—C30—C351.1 (5)
P3—C49—C50—C51177.2 (3)C32—C33—C34—C350.2 (7)
P3—C49—C54—C53176.4 (3)C35—C30—P2—C3670.7 (3)
P4—Mn4—Mn3—C9161.6 (12)C36—C37—C38—C391.7 (6)
P4—Mn4—Mn3—C10150.28 (14)C36—C41—C40—C390.6 (6)
P4—Mn4—Mn3—C1163.08 (11)C37—C36—C41—C400.6 (5)
P4—Mn4—Mn3—C12119.08 (11)C37—C38—C39—C400.5 (7)
P4—C42—P3—C43115.90 (17)C38—C37—C36—C411.7 (5)
P4—C42—P3—C49141.06 (16)C38—C39—C40—C410.6 (7)
P4—C55—C56—C57178.9 (3)C42—P3—C43—C44128.3 (3)
P4—C55—C60—C59177.5 (3)C42—P3—C43—C4851.3 (3)
P4—C61—C62—C63177.9 (3)C42—P3—C49—C50151.5 (3)
P4—C61—C66—C65178.3 (3)C42—P3—C49—C5432.2 (3)
C1—Mn1—P1—C17171.72 (15)C42—P4—C55—C56174.9 (2)
C1—Mn1—P1—C1850.21 (15)C42—P4—C55—C604.9 (3)
C1—Mn1—P1—C2468.61 (15)C42—P4—C61—C6277.2 (3)
C2—Mn1—Mn2—C5110.0 (18)C42—P4—C61—C66100.5 (3)
C2—Mn1—Mn2—C629.40 (17)C43—P3—C49—C5046.9 (3)
C2—Mn1—Mn2—C758.55 (16)C43—P3—C49—C54136.8 (3)
C2—Mn1—Mn2—C8116.87 (16)C43—C44—C45—C460.4 (6)
C3—Mn1—Mn2—C522.0 (18)C43—C48—C47—C460.6 (6)
C3—Mn1—Mn2—C6117.45 (16)C44—C43—P3—C49125.1 (3)
C3—Mn1—Mn2—C729.50 (15)C44—C43—C48—C471.2 (5)
C3—Mn1—Mn2—C8155.08 (15)C44—C45—C46—C471.0 (7)
C3—Mn1—P1—C1776.83 (15)C45—C44—C43—C480.7 (5)
C3—Mn1—P1—C1844.69 (15)C45—C46—C47—C480.5 (6)
C3—Mn1—P1—C24163.51 (15)C48—C43—P3—C4955.2 (3)
C4—Mn1—Mn2—C5159.8 (18)C49—C50—C51—C520.9 (6)
C4—Mn1—Mn2—C660.73 (16)C49—C54—C53—C520.2 (6)
C4—Mn1—Mn2—C7148.67 (15)C50—C49—C54—C530.2 (6)
C4—Mn1—Mn2—C826.74 (15)C50—C51—C52—C530.4 (7)
C4—Mn1—P1—C1796.08 (15)C51—C50—C49—C540.8 (6)
C4—Mn1—P1—C18142.40 (15)C51—C52—C53—C540.1 (7)
C4—Mn1—P1—C2423.59 (15)C55—P4—C61—C62173.0 (3)
C5—Mn2—P2—C17140.31 (14)C55—P4—C61—C669.3 (3)
C5—Mn2—P2—C3094.17 (15)C55—C56—C57—C580.0 (6)
C5—Mn2—P2—C3626.36 (15)C55—C60—C59—C582.9 (6)
C7—Mn2—P2—C17123.71 (14)C56—C55—P4—C6171.8 (3)
C7—Mn2—P2—C301.81 (15)C56—C55—C60—C592.7 (5)
C7—Mn2—P2—C36122.34 (15)C56—C57—C58—C590.2 (7)
C8—Mn2—P2—C1744.69 (14)C57—C56—C55—C601.3 (5)
C8—Mn2—P2—C30170.20 (15)C57—C58—C59—C601.7 (7)
C8—Mn2—P2—C3669.27 (15)C60—C55—P4—C61108.0 (3)
C9—Mn3—P3—C42171.78 (16)C61—C62—C63—C640.1 (7)
C9—Mn3—P3—C4350.18 (17)C61—C66—C65—C641.1 (7)
C9—Mn3—P3—C4968.09 (17)C62—C61—C66—C650.6 (6)
C10—Mn3—Mn4—C13107.7 (14)C62—C63—C64—C650.6 (7)
C10—Mn3—Mn4—C1432.05 (18)C63—C62—C61—C660.1 (6)
C10—Mn3—Mn4—C1556.41 (17)C63—C64—C65—C661.1 (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) x1, y, z; (ix) x, y, z+1.
(II) µ-Bis(diphenylphosphino)methane-P:P'-octacarbonyldimanganese(Mn—Mn) toluene hemisolvate top
Crystal data top
[Mn2(CO)8(C25H22P2)]·0.5C7H8Dx = 1.469 Mg m3
Mr = 764.43Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41cdCell parameters from 25 reflections
Hall symbol: I 41b -2cθ = 15.5–16.0°
a = 18.286 (2) ŵ = 0.87 mm1
c = 41.345 (6) ÅT = 294 K
V = 13824 (3) Å3Block, yellow
Z = 160.36 × 0.32 × 0.29 mm
F(000) = 6224.00
Data collection top
Enraf-Nonius CAD-4
diffractometer
2520 reflections with I > 1σ(I)
Radiation source: sealed X-ray tubeRint = 0.000
Graphite monochromatorθmax = 25.0°, θmin = 1.6°
ω scansh = 021
Absorption correction: ψ-scan
(North et al., 1968)
k = 015
Tmin = 0.72, Tmax = 0.77l = 049
3084 measured reflections3 standard reflections every 60 min
3084 independent reflections intensity decay: 1.1%
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.038 w = 4Fo2/[σ2(I) + (0.02I)2]
S = 1.32(Δ/σ)max = 0.005
3084 reflectionsΔρmax = 0.48 e Å3
438 parametersΔρmin = 0.48 e Å3
Crystal data top
[Mn2(CO)8(C25H22P2)]·0.5C7H8Z = 16
Mr = 764.43Mo Kα radiation
Tetragonal, I41cdµ = 0.87 mm1
a = 18.286 (2) ÅT = 294 K
c = 41.345 (6) Å0.36 × 0.32 × 0.29 mm
V = 13824 (3) Å3
Data collection top
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 = 0.773 standard reflections every 60 min
3084 measured reflections intensity decay: 1.1%
3084 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.038H-atom parameters constrained
S = 1.32Δρmax = 0.48 e Å3
3084 reflectionsΔρmin = 0.48 e Å3
438 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.68920 (5)0.64484 (5)0.50000.0407 (3)
Mn20.60238 (5)0.63975 (5)0.55966 (3)0.0423 (3)
P10.64564 (9)0.76189 (9)0.49097 (5)0.0368 (5)
P20.62335 (9)0.76355 (9)0.56508 (5)0.0372 (5)
O10.7646 (3)0.6396 (3)0.43734 (13)0.0691 (19)
O20.5559 (3)0.5771 (3)0.47107 (16)0.082 (2)
O30.7437 (3)0.4977 (3)0.51898 (14)0.0719 (18)
O40.8217 (3)0.6932 (3)0.53497 (13)0.0661 (19)
O50.4660 (3)0.6708 (3)0.52227 (13)0.0621 (18)
O60.5775 (3)0.4832 (3)0.5466 (2)0.100 (3)
O70.7452 (3)0.5935 (3)0.58729 (13)0.0612 (17)
O80.5286 (3)0.6288 (4)0.62228 (16)0.096 (2)
C10.7347 (4)0.6432 (4)0.46202 (18)0.047 (2)
C20.6059 (5)0.6045 (4)0.48308 (19)0.059 (3)
C30.7212 (4)0.5536 (4)0.51171 (18)0.051 (2)
C40.7675 (4)0.6781 (4)0.52275 (16)0.044 (2)
C50.5198 (5)0.6602 (4)0.53607 (18)0.051 (2)
C60.5877 (4)0.5436 (4)0.5513 (2)0.063 (3)
C70.6914 (4)0.6143 (4)0.57623 (18)0.046 (2)
C80.5571 (4)0.6344 (4)0.5978 (2)0.059 (3)
C90.6160 (4)0.8131 (4)0.52706 (17)0.047 (2)
C100.5679 (3)0.7658 (4)0.46352 (16)0.0386 (19)
C110.4998 (4)0.7940 (4)0.47055 (19)0.063 (2)
C120.4432 (5)0.7943 (6)0.4482 (3)0.084 (4)
C130.4556 (5)0.7673 (6)0.4180 (3)0.078 (3)
C140.5226 (5)0.7392 (6)0.4103 (2)0.077 (3)
C150.5774 (4)0.7376 (5)0.43250 (19)0.060 (3)
C160.5576 (4)0.8158 (4)0.58945 (16)0.0385 (19)
C170.5796 (4)0.8641 (4)0.61387 (18)0.052 (2)
C180.5284 (5)0.9045 (4)0.6310 (2)0.065 (3)
C190.4550 (5)0.8968 (5)0.6248 (2)0.062 (3)
C200.4335 (4)0.8496 (5)0.6013 (2)0.063 (3)
C210.4832 (4)0.8087 (4)0.58377 (19)0.057 (3)
C220.7101 (4)0.7896 (3)0.58353 (16)0.0378 (19)
C230.7266 (4)0.7578 (4)0.61303 (16)0.049 (2)
C240.7910 (5)0.7750 (5)0.62854 (19)0.065 (3)
C250.8398 (5)0.8220 (6)0.6148 (3)0.082 (4)
C260.8251 (5)0.8518 (5)0.5860 (3)0.078 (3)
C270.7605 (4)0.8378 (4)0.56902 (18)0.062 (3)
C280.7071 (4)0.8288 (4)0.47190 (16)0.0387 (19)
C290.7825 (4)0.8227 (4)0.4744 (2)0.062 (3)
C300.8276 (4)0.8761 (5)0.4616 (2)0.071 (3)
C310.7984 (6)0.9349 (5)0.4464 (2)0.069 (3)
C320.7240 (6)0.9407 (4)0.4428 (2)0.069 (3)
C330.6787 (4)0.8877 (4)0.45615 (18)0.050 (2)
C340.50000.50000.7941 (4)0.088 (5)
C350.4766 (5)0.4415 (5)0.7763 (3)0.090 (4)
C360.4762 (5)0.4399 (5)0.7431 (3)0.080 (3)
C370.50000.50000.7248 (4)0.075 (4)
C380.50000.50000.6887 (3)0.112 (6)
H10.64510.85590.52860.057*
H20.56620.82650.52410.057*
H30.49140.81400.49140.075*
H40.39650.81310.45390.100*
H50.41770.76790.40240.094*
H60.53090.72060.38910.093*
H70.62320.71680.42680.072*
H80.63010.86920.61870.062*
H90.54420.93770.64730.078*
H100.41980.92400.63660.074*
H110.38290.84450.59670.075*
H120.46640.77540.56780.068*
H130.69350.72410.62260.059*
H140.80140.75380.64900.078*
H150.88410.83360.62570.098*
H160.86000.88400.57670.094*
H170.75100.85970.54860.075*
H180.80330.78150.48500.074*
H190.87920.87150.46360.085*
H200.82940.97210.43810.082*
H210.70370.98070.43120.083*
H220.62710.89270.45430.060*
H230.50000.50000.81710.106*
H240.45950.39950.78750.108*
H260.45960.39730.73220.096*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0417 (6)0.0370 (6)0.0434 (6)0.0029 (5)0.0055 (5)0.0002 (5)
Mn20.0394 (6)0.0388 (6)0.0489 (6)0.0045 (5)0.0027 (5)0.0064 (6)
P10.0386 (10)0.0383 (10)0.0336 (9)0.0032 (8)0.0021 (8)0.0012 (8)
P20.0394 (10)0.0402 (10)0.0321 (9)0.0021 (8)0.0030 (8)0.0041 (8)
O10.072 (4)0.080 (4)0.055 (3)0.008 (3)0.013 (3)0.007 (3)
O20.064 (4)0.085 (5)0.097 (5)0.015 (3)0.020 (4)0.017 (4)
O30.095 (4)0.038 (3)0.083 (4)0.014 (3)0.007 (4)0.010 (3)
O40.056 (3)0.071 (4)0.072 (4)0.002 (3)0.016 (3)0.003 (3)
O50.054 (3)0.064 (4)0.068 (4)0.000 (3)0.017 (3)0.009 (3)
O60.069 (4)0.034 (3)0.196 (8)0.013 (3)0.031 (5)0.008 (4)
O70.054 (3)0.066 (4)0.063 (3)0.008 (3)0.011 (3)0.010 (3)
O80.084 (5)0.131 (6)0.073 (4)0.013 (4)0.029 (4)0.043 (4)
C10.047 (4)0.046 (4)0.048 (5)0.003 (4)0.011 (4)0.001 (4)
C20.074 (6)0.040 (5)0.062 (6)0.010 (4)0.003 (5)0.002 (4)
C30.055 (5)0.048 (5)0.049 (5)0.007 (4)0.009 (4)0.005 (4)
C40.054 (5)0.041 (4)0.038 (4)0.010 (4)0.006 (4)0.006 (3)
C50.057 (5)0.037 (4)0.058 (5)0.007 (4)0.001 (4)0.004 (4)
C60.045 (5)0.052 (5)0.091 (7)0.006 (4)0.017 (5)0.019 (5)
C70.045 (5)0.047 (4)0.045 (4)0.006 (4)0.005 (4)0.006 (4)
C80.058 (5)0.050 (5)0.069 (6)0.002 (4)0.002 (5)0.016 (5)
C90.063 (5)0.036 (4)0.043 (4)0.003 (4)0.002 (4)0.000 (3)
C100.035 (4)0.045 (4)0.036 (4)0.005 (3)0.002 (3)0.005 (3)
C110.043 (4)0.079 (5)0.066 (5)0.015 (4)0.003 (5)0.004 (5)
C120.044 (5)0.118 (9)0.089 (7)0.019 (5)0.016 (5)0.005 (7)
C130.056 (6)0.097 (7)0.082 (7)0.004 (5)0.035 (6)0.010 (6)
C140.080 (7)0.106 (8)0.046 (5)0.001 (6)0.023 (5)0.008 (5)
C150.050 (5)0.078 (6)0.052 (5)0.008 (4)0.006 (4)0.001 (5)
C160.045 (4)0.039 (4)0.031 (4)0.004 (3)0.002 (3)0.003 (3)
C170.050 (4)0.059 (5)0.047 (5)0.008 (4)0.000 (4)0.000 (4)
C180.076 (6)0.053 (5)0.067 (6)0.003 (5)0.003 (5)0.018 (5)
C190.063 (6)0.057 (5)0.065 (6)0.002 (5)0.016 (5)0.004 (5)
C200.041 (4)0.061 (5)0.087 (6)0.002 (4)0.005 (5)0.011 (5)
C210.052 (5)0.054 (5)0.064 (5)0.000 (4)0.000 (4)0.016 (4)
C220.046 (4)0.035 (4)0.033 (4)0.000 (3)0.003 (3)0.009 (3)
C230.049 (4)0.056 (5)0.041 (4)0.000 (4)0.003 (4)0.012 (4)
C240.060 (5)0.078 (6)0.056 (6)0.000 (5)0.018 (4)0.015 (5)
C250.054 (6)0.106 (8)0.085 (7)0.006 (6)0.019 (5)0.025 (7)
C260.050 (5)0.092 (7)0.092 (7)0.036 (5)0.016 (5)0.005 (6)
C270.067 (5)0.067 (5)0.053 (5)0.030 (4)0.014 (4)0.002 (4)
C280.041 (4)0.037 (4)0.038 (4)0.001 (3)0.008 (3)0.009 (3)
C290.051 (5)0.064 (5)0.070 (6)0.000 (4)0.005 (4)0.010 (5)
C300.052 (5)0.071 (6)0.089 (7)0.014 (5)0.022 (5)0.005 (5)
C310.092 (7)0.058 (6)0.055 (6)0.026 (5)0.020 (5)0.005 (5)
C320.102 (8)0.043 (5)0.062 (6)0.014 (5)0.010 (5)0.004 (4)
C330.056 (5)0.043 (4)0.050 (5)0.004 (4)0.007 (4)0.004 (4)
C340.073 (9)0.105 (11)0.088 (11)0.001 (9)0.00000.0000
C350.079 (8)0.086 (7)0.105 (9)0.005 (6)0.013 (7)0.011 (7)
C360.066 (6)0.074 (6)0.100 (8)0.007 (5)0.000 (6)0.021 (6)
C370.067 (8)0.062 (8)0.096 (11)0.022 (7)0.00000.0000
C380.107 (12)0.164 (16)0.067 (9)0.047 (12)0.00000.0000
Geometric parameters (Å, º) top
Mn1—Mn22.9338 (14)C17—C181.388 (10)
Mn1—P12.314 (2)C17—H80.95
Mn1—C11.778 (8)C18—C191.374 (11)
Mn1—C21.832 (9)C18—H90.95
Mn1—C31.833 (8)C19—C201.357 (11)
Mn1—C41.817 (8)C19—H100.95
Mn2—P22.307 (2)C20—C211.382 (10)
Mn2—C51.836 (9)C20—H110.95
Mn2—C61.812 (8)C21—H120.95
Mn2—C71.827 (7)C22—C231.385 (9)
Mn2—C81.782 (9)C22—C271.409 (9)
P1—C91.843 (7)C23—C241.376 (10)
P1—C101.821 (6)C23—H130.95
P1—C281.839 (7)C24—C251.365 (12)
P2—C91.820 (7)C24—H140.95
P2—C161.837 (7)C25—C261.338 (13)
P2—C221.824 (7)C25—H150.95
O1—C11.160 (8)C26—C271.397 (11)
O2—C21.154 (9)C26—H160.95
O3—C31.142 (8)C27—H170.95
O4—C41.147 (8)C28—C291.387 (9)
O5—C51.153 (8)C28—C331.362 (9)
O6—C61.136 (8)C29—C301.382 (10)
O7—C71.149 (8)C29—H180.95
O8—C81.144 (9)C30—C311.357 (11)
C9—H10.95C30—H190.95
C9—H20.95C31—C321.371 (12)
C10—C111.378 (9)C31—H200.95
C10—C151.393 (9)C32—C331.389 (10)
C11—C121.388 (11)C32—H210.95
C11—H30.95C33—H220.95
C12—C131.360 (13)C34—C351.368 (12)
C12—H40.95C34—C35i1.368 (12)
C13—C141.366 (12)C34—H230.95
C13—H50.95C35—C361.373 (13)
C14—C151.361 (10)C35—H240.95
C14—H60.95C36—C371.401 (12)
C15—H70.95C36—H260.95
C16—C171.400 (9)C37—C381.496 (18)
C16—C211.386 (9)
O1···C23ii3.484 (9)O6···O6i2.901 (12)
O1···C12iii3.512 (10)O6···C6i3.067 (9)
O2···O2i3.484 (12)O6···C5i3.199 (9)
O3···C32iv3.370 (10)O6···C26iv3.406 (10)
O3···C30iv3.503 (10)O7···C13v3.465 (11)
O3···C33iv3.579 (9)O8···C25vi3.579 (11)
O3···C27iv3.583 (9)C3···C31iv3.484 (11)
O4···C20iii3.508 (10)C6···C6i3.582 (15)
O4···C21iii3.577 (9)C19···C31vii3.484 (12)
O5···O6i3.094 (8)O(6)···C(6)i3.067 (9)
Mn2—Mn1—P188.80 (6)C15—C14—H6119.7
Mn2—Mn1—C1174.4 (2)C10—C15—C14121.4 (7)
Mn2—Mn1—C281.9 (3)C10—C15—H7119.3
Mn2—Mn1—C385.5 (3)C14—C15—H7119.3
Mn2—Mn1—C490.2 (2)P2—C16—C17122.4 (5)
P1—Mn1—C191.9 (2)P2—C16—C21120.0 (5)
P1—Mn1—C291.4 (2)C17—C16—C21117.6 (7)
P1—Mn1—C3173.9 (3)C16—C17—C18120.7 (7)
P1—Mn1—C492.6 (2)C16—C17—H8119.6
C1—Mn1—C292.5 (3)C18—C17—H8119.7
C1—Mn1—C393.9 (3)C17—C18—C19120.5 (8)
C1—Mn1—C495.4 (3)C17—C18—H9119.8
C2—Mn1—C390.0 (3)C19—C18—H9119.8
C2—Mn1—C4171.0 (3)C18—C19—C20118.9 (8)
C3—Mn1—C485.3 (3)C18—C19—H10120.6
Mn1—Mn2—P287.74 (6)C20—C19—H10120.6
Mn1—Mn2—C589.5 (2)C19—C20—C21121.9 (7)
Mn1—Mn2—C687.2 (3)C19—C20—H11119.0
Mn1—Mn2—C780.8 (2)C21—C20—H11119.0
Mn1—Mn2—C8174.8 (2)C16—C21—C20120.4 (7)
P2—Mn2—C589.3 (2)C16—C21—H12119.8
P2—Mn2—C6174.5 (3)C20—C21—H12119.8
P2—Mn2—C793.7 (2)P2—C22—C23116.6 (5)
P2—Mn2—C892.6 (3)P2—C22—C27123.7 (5)
C5—Mn2—C688.5 (3)C23—C22—C27119.6 (7)
C5—Mn2—C7169.8 (3)C22—C23—C24120.1 (7)
C5—Mn2—C895.7 (3)C22—C23—H13120.0
C6—Mn2—C787.5 (3)C24—C23—H13119.9
C6—Mn2—C892.7 (4)C23—C24—C25120.7 (8)
C7—Mn2—C893.9 (3)C23—C24—H14119.7
Mn1—P1—C9116.1 (2)C25—C24—H14119.7
Mn1—P1—C10113.9 (2)C24—C25—C26119.7 (8)
Mn1—P1—C28118.3 (2)C24—C25—H15120.2
C9—P1—C10104.8 (3)C26—C25—H15120.2
C9—P1—C28100.9 (3)C25—C26—C27122.9 (8)
C10—P1—C28100.6 (3)C25—C26—H16118.6
Mn2—P2—C9113.1 (2)C27—C26—H16118.6
Mn2—P2—C16117.1 (2)C22—C27—C26117.0 (7)
Mn2—P2—C22116.2 (2)C22—C27—H17121.5
C9—P2—C1699.6 (3)C26—C27—H17121.5
C9—P2—C22107.2 (3)P1—C28—C29121.5 (6)
C16—P2—C22101.8 (3)P1—C28—C33119.9 (5)
Mn1—C1—O1177.6 (7)C29—C28—C33118.6 (7)
Mn1—C2—O2176.0 (7)C28—C29—C30120.5 (8)
Mn1—C3—O3177.4 (7)C28—C29—H18119.8
Mn1—C4—O4171.8 (6)C30—C29—H18119.8
Mn2—C5—O5176.6 (6)C29—C30—C31120.2 (8)
Mn2—C6—O6178.6 (9)C29—C30—H19119.9
Mn2—C7—O7174.9 (7)C31—C30—H19119.9
Mn2—C8—O8178.1 (8)C30—C31—C32120.1 (8)
P1—C9—P2115.1 (4)C30—C31—H20120.0
P1—C9—H1108.0C32—C31—H20120.0
P1—C9—H2108.0C31—C32—C33119.7 (8)
P2—C9—H1108.0C31—C32—H21120.1
P2—C9—H2108.0C33—C32—H21120.1
H1—C9—H2109.5C28—C33—C32120.9 (7)
P1—C10—C11126.0 (6)C28—C33—H22119.6
P1—C10—C15117.5 (5)C32—C33—H22119.6
C11—C10—C15116.5 (6)C35—C34—C35i114.6 (14)
C10—C11—C12122.3 (8)C35—C34—H23122.7
C10—C11—H3118.8C35i—C34—H23122.7
C12—C11—H3118.8C34—C35—C36123.9 (11)
C11—C12—C13119.0 (8)C34—C35—H24118.0
C11—C12—H4120.5C36—C35—H24118.0
C13—C12—H4120.5C35—C36—C37121.3 (10)
C12—C13—C14120.2 (8)C35—C36—H26119.3
C12—C13—H5119.9C37—C36—H26119.3
C14—C13—H5119.9C36—C37—C36i114.9 (13)
C13—C14—C15120.6 (8)C36—C37—C38122.5 (6)
C13—C14—H6119.7C36i—C37—C38122.5 (6)
Mn1—Mn2—P2—C941.7 (3)C4—Mn1—P1—C10172.9 (3)
Mn1—Mn2—P2—C16156.6 (2)C4—Mn1—P1—C2855.0 (3)
Mn1—Mn2—P2—C2282.9 (2)C5—Mn2—P2—C947.9 (4)
Mn1—P1—C9—P21.2 (5)C5—Mn2—P2—C1667.0 (3)
Mn1—P1—C10—C11121.3 (6)C5—Mn2—P2—C22172.5 (3)
Mn1—P1—C10—C1558.5 (6)C7—Mn2—P2—C9122.4 (4)
Mn1—P1—C28—C2925.8 (7)C7—Mn2—P2—C16122.7 (3)
Mn1—P1—C28—C33157.3 (5)C7—Mn2—P2—C222.3 (3)
Mn2—Mn1—P1—C924.9 (3)C8—Mn2—P2—C9143.6 (4)
Mn2—Mn1—P1—C1097.0 (2)C8—Mn2—P2—C1628.7 (3)
Mn2—Mn1—P1—C28145.1 (2)C8—Mn2—P2—C2291.8 (3)
Mn2—P2—C9—P133.4 (5)C9—P1—C10—C116.6 (7)
Mn2—P2—C16—C17130.9 (5)C9—P1—C10—C15173.5 (6)
Mn2—P2—C16—C2149.6 (7)C9—P1—C28—C29102.0 (7)
Mn2—P2—C22—C2352.5 (6)C9—P1—C28—C3375.0 (6)
Mn2—P2—C22—C27125.7 (6)C9—P2—C16—C17106.8 (6)
P1—Mn1—Mn2—P233.25 (7)C9—P2—C16—C2172.6 (6)
P1—Mn1—Mn2—C556.1 (2)C9—P2—C22—C23180.0 (5)
P1—Mn1—Mn2—C6144.7 (2)C9—P2—C22—C271.9 (7)
P1—Mn1—Mn2—C7127.4 (2)C10—P1—C28—C29150.5 (6)
P1—Mn1—Mn2—C8127 (3)C10—P1—C28—C3332.5 (6)
P1—C9—P2—C16158.4 (4)C10—C11—C12—C131.4 (14)
P1—C9—P2—C2296.0 (4)C10—C15—C14—C131.5 (15)
P1—C10—C11—C12179.5 (7)C11—C10—P1—C28111.0 (7)
P1—C10—C15—C14179.0 (7)C11—C10—C15—C141.1 (12)
P1—C28—C29—C30175.9 (6)C11—C12—C13—C141.1 (16)
P1—C28—C33—C32177.2 (6)C12—C11—C10—C150.3 (12)
P2—Mn2—Mn1—C1131 (2)C12—C13—C14—C150.3 (16)
P2—Mn2—Mn1—C2124.8 (2)C15—C10—P1—C2869.2 (6)
P2—Mn2—Mn1—C3144.6 (2)C16—P2—C22—C2375.9 (6)
P2—Mn2—Mn1—C459.3 (2)C16—P2—C22—C27105.9 (6)
P2—C9—P1—C10125.4 (4)C16—C17—C18—C191.2 (13)
P2—C9—P1—C28130.4 (4)C16—C21—C20—C191.2 (13)
P2—C16—C17—C18177.8 (6)C17—C16—P2—C223.1 (6)
P2—C16—C21—C20177.9 (6)C17—C16—C21—C201.6 (11)
P2—C22—C23—C24179.7 (6)C17—C18—C19—C200.7 (14)
P2—C22—C27—C26179.3 (6)C18—C17—C16—C211.7 (11)
C1—Mn1—P1—C9160.6 (3)C18—C19—C20—C210.7 (13)
C1—Mn1—P1—C1077.5 (3)C21—C16—P2—C22177.4 (6)
C1—Mn1—P1—C2840.4 (3)C22—C23—C24—C251.5 (13)
C2—Mn1—Mn2—C535.5 (3)C22—C27—C26—C250.3 (14)
C2—Mn1—Mn2—C653.1 (3)C23—C22—C27—C261.2 (11)
C2—Mn1—Mn2—C7141.0 (3)C23—C24—C25—C260.0 (15)
C2—Mn1—Mn2—C8141 (3)C24—C23—C22—C272.0 (11)
C2—Mn1—P1—C9106.8 (4)C24—C25—C26—C270.9 (16)
C2—Mn1—P1—C1015.1 (3)C28—C29—C30—C310.3 (14)
C2—Mn1—P1—C28133.0 (3)C28—C33—C32—C312.1 (12)
C3—Mn1—Mn2—C5126.1 (3)C29—C28—C33—C320.1 (11)
C3—Mn1—Mn2—C637.5 (3)C29—C30—C31—C321.7 (14)
C3—Mn1—Mn2—C750.4 (3)C30—C29—C28—C331.1 (12)
C3—Mn1—Mn2—C851 (3)C30—C31—C32—C332.9 (13)
C4—Mn1—Mn2—C5148.7 (3)C34—C35—C36—C370.5 (14)
C4—Mn1—Mn2—C6122.8 (3)C34—C35i—C36i—C370.5 (14)
C4—Mn1—Mn2—C734.8 (3)C35—C34—C35i—C36i0.3 (7)
C4—Mn1—Mn2—C835 (3)C35—C36—C37—C36i0.2 (7)
C4—Mn1—P1—C965.2 (4)C35—C36—C37—C38179.8 (7)
Symmetry codes: (i) x+1, y+1, z; (ii) y+3/2, x, z1/4; (iii) x+1/2, y+3/2, z; (iv) x+3/2, y1/2, z; (v) y+3/2, x+1, z+1/4; (vi) x1/2, y+3/2, z; (vii) y1/2, x, z+1/4.

Experimental details

(I)(II)
Crystal data
Chemical formula[Mn2(CO)8(C25H22P2)][Mn2(CO)8(C25H22P2)]·0.5C7H8
Mr718.36764.43
Crystal system, space groupTriclinic, P1Tetragonal, I41cd
Temperature (K)296294
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
V3)3207 (2)13824 (3)
Z416
Radiation typeMo KαMo Kα
µ (mm1)0.940.87
Crystal size (mm)0.40 × 0.20 × 0.050.36 × 0.32 × 0.29
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Enraf-Nonius CAD-4
diffractometer
Absorption correctionAnalytical
(de Meulenaer & Tompa, 1965)
ψ-scan
(North et al., 1968)
Tmin, Tmax0.763, 0.9580.72, 0.77
No. of measured, independent and
observed reflections
11815, 11243, 8260 [I > σ(I)]3084, 3084, 2520 [I > 1σ(I)]
Rint0.0210.000
(sin θ/λ)max1)0.5950.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.044, 1.40 0.045, 0.038, 1.32
No. of reflections112433084
No. of parameters811438
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.47, 0.460.48, 0.48

Computer programs: CAD-4-PC Software (Enraf-Nonius, 1993), CAD-4-PC Software, TEXSAN (Molecular Structure Corporation, 1997), TEXSAN.

Selected geometric parameters (Å, º) for (I) top
Mn1—Mn22.9746 (7)Mn3—Mn42.9714 (7)
Mn1—P12.3033 (9)Mn3—P32.3039 (9)
Mn1—C11.788 (4)Mn3—C91.784 (4)
Mn1—C21.832 (4)Mn3—C101.815 (4)
Mn1—C31.844 (4)Mn3—C111.844 (4)
Mn1—C41.840 (4)Mn3—C121.836 (4)
Mn2—P22.3020 (9)Mn4—P42.3028 (9)
Mn2—C51.788 (4)Mn4—C131.781 (4)
Mn2—C61.814 (4)Mn4—C141.820 (4)
Mn2—C71.842 (4)Mn4—C151.854 (4)
Mn2—C81.827 (4)Mn4—C161.827 (4)
Mn2—Mn1—P192.17 (3)Mn4—Mn3—P391.58 (3)
Mn2—Mn1—C1175.32 (11)Mn4—Mn3—C9173.93 (12)
Mn2—Mn1—C284.37 (11)Mn4—Mn3—C1083.89 (13)
Mn2—Mn1—C388.25 (10)Mn4—Mn3—C1190.51 (11)
Mn2—Mn1—C484.58 (10)Mn4—Mn3—C1283.80 (12)
P1—Mn1—C191.25 (12)P3—Mn3—C992.57 (12)
P1—Mn1—C2176.48 (11)P3—Mn3—C10175.30 (13)
P1—Mn1—C391.39 (11)P3—Mn3—C1191.51 (11)
P1—Mn1—C490.70 (11)P3—Mn3—C1290.80 (11)
C1—Mn1—C292.24 (16)C9—Mn3—C1092.04 (17)
C1—Mn1—C394.87 (14)C9—Mn3—C1193.81 (16)
C1—Mn1—C492.18 (15)C9—Mn3—C1291.71 (17)
C2—Mn1—C387.89 (16)C10—Mn3—C1187.27 (17)
C2—Mn1—C489.60 (16)C10—Mn3—C1289.98 (17)
C3—Mn1—C4172.60 (15)C11—Mn3—C12173.92 (16)
Mn1—Mn2—P286.17 (3)Mn3—Mn4—P486.09 (3)
Mn1—Mn2—C5176.71 (11)Mn3—Mn4—C13175.71 (11)
Mn1—Mn2—C690.71 (12)Mn3—Mn4—C1491.53 (12)
Mn1—Mn2—C782.06 (10)Mn3—Mn4—C1581.11 (11)
Mn1—Mn2—C886.63 (10)Mn3—Mn4—C1687.43 (10)
P2—Mn2—C591.40 (11)P4—Mn4—C1390.75 (11)
P2—Mn2—C6176.38 (12)P4—Mn4—C14176.67 (12)
P2—Mn2—C793.32 (11)P4—Mn4—C1593.21 (10)
P2—Mn2—C890.46 (10)P4—Mn4—C1690.28 (10)
C5—Mn2—C691.79 (16)C13—Mn4—C1491.75 (16)
C5—Mn2—C795.89 (14)C13—Mn4—C1596.19 (15)
C5—Mn2—C895.61 (14)C13—Mn4—C1695.49 (15)
C6—Mn2—C788.07 (16)C14—Mn4—C1588.71 (15)
C6—Mn2—C887.52 (16)C14—Mn4—C1687.29 (15)
C7—Mn2—C8167.80 (14)C15—Mn4—C16167.76 (15)
P1—Mn1—Mn2—P226.93 (3)P3—Mn3—Mn4—P428.44 (3)
Selected geometric parameters (Å, º) for (II) top
Mn1—Mn22.9338 (14)Mn2—P22.307 (2)
Mn1—P12.314 (2)Mn2—C51.836 (9)
Mn1—C11.778 (8)Mn2—C61.812 (8)
Mn1—C21.832 (9)Mn2—C71.827 (7)
Mn1—C31.833 (8)Mn2—C81.782 (9)
Mn1—C41.817 (8)
Mn2—Mn1—P188.80 (6)Mn1—Mn2—P287.74 (6)
Mn2—Mn1—C1174.4 (2)Mn1—Mn2—C589.5 (2)
Mn2—Mn1—C281.9 (3)Mn1—Mn2—C687.2 (3)
Mn2—Mn1—C385.5 (3)Mn1—Mn2—C780.8 (2)
Mn2—Mn1—C490.2 (2)Mn1—Mn2—C8174.8 (2)
P1—Mn1—C191.9 (2)P2—Mn2—C589.3 (2)
P1—Mn1—C291.4 (2)P2—Mn2—C6174.5 (3)
P1—Mn1—C3173.9 (3)P2—Mn2—C793.7 (2)
P1—Mn1—C492.6 (2)P2—Mn2—C892.6 (3)
C1—Mn1—C292.5 (3)C5—Mn2—C688.5 (3)
C1—Mn1—C393.9 (3)C5—Mn2—C7169.8 (3)
C1—Mn1—C495.4 (3)C5—Mn2—C895.7 (3)
C2—Mn1—C390.0 (3)C6—Mn2—C787.5 (3)
C2—Mn1—C4171.0 (3)C6—Mn2—C892.7 (4)
C3—Mn1—C485.3 (3)C7—Mn2—C893.9 (3)
P1—Mn1—Mn2—P233.25 (7)
 

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