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The title compound, [Mn2(C8H6P)(C14H11P)(CO)8], displays a novel coordination mode for a phospho­lyl ligand, where dinuclear coordination is observed through the P atom and the adjacent C atom of the heterocycle.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804030892/bv6005sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804030892/bv6005Isup2.hkl
Contains datablock I

CCDC reference: 259089

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.011 Å
  • R factor = 0.072
  • wR factor = 0.181
  • Data-to-parameter ratio = 13.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.37 PLAT230_ALERT_2_C Hirshfeld Test Diff for O14 - C14 .. 5.62 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn2 - C14 .. 6.26 su PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997–1999); cell refinement: SMART; data reduction: SAINT (Bruker, 1997–2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: SHELXTL (Sheldrick, 1997a); software used to prepare material for publication: SHELXTL.

2-phosphindolyl)(µ2-1-phenyl-phosphind-2-yl-C,P)bis(manganese- tetracarbonyl) top
Crystal data top
[Mn2(C8H6P)(C14H11P)(CO)8]F(000) = 2720
Mr = 676.25Dx = 1.571 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4864 reflections
a = 20.681 (2) Åθ = 2.2–30.5°
b = 9.8850 (9) ŵ = 1.05 mm1
c = 28.440 (2) ÅT = 173 K
β = 100.368 (4)°Irregular, orange
V = 5719.2 (9) Å30.25 × 0.15 × 0.10 mm
Z = 8
Data collection top
CCD area detector
diffractometer
5036 independent reflections
Radiation source: fine-focus sealed tube, Bruker AXS SMART 100/P42916 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
ω and φ scansθmax = 25.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997a)
h = 2424
Tmin = 0.765, Tmax = 0.903k = 1111
18319 measured reflectionsl = 3333
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.072Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.181H-atom parameters constrained
S = 0.97 w = 1/[σ2(Fo2) + (0.097P)2]
where P = (Fo2 + 2Fc2)/3
5036 reflections(Δ/σ)max < 0.001
379 parametersΔρmax = 1.21 e Å3
0 restraintsΔρmin = 0.51 e Å3
Special details top

Experimental. Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.25207 (5)0.21645 (11)0.14302 (3)0.0384 (3)
Mn20.22930 (5)0.16312 (10)0.08593 (4)0.0399 (3)
P10.18078 (8)0.04752 (18)0.10083 (6)0.0359 (4)
P20.33336 (9)0.05168 (19)0.15169 (6)0.0392 (5)
C20.1365 (4)0.1187 (7)0.0451 (2)0.0434 (18)
H2A0.15660.14530.01990.052*
C30.0723 (4)0.1284 (7)0.0445 (3)0.0467 (18)
H3A0.04300.16030.01820.056*
C3A0.0514 (4)0.0857 (7)0.0880 (2)0.0434 (17)
C40.0133 (4)0.0869 (7)0.0977 (3)0.056 (2)
H4A0.04820.11700.07470.067*
C50.0239 (4)0.0426 (8)0.1419 (3)0.062 (2)
H5A0.06610.04520.14900.074*
C60.0267 (4)0.0047 (8)0.1749 (3)0.057 (2)
H6A0.01840.03360.20430.068*
C70.0905 (4)0.0113 (7)0.1662 (2)0.0463 (18)
H7A0.12420.04700.18890.056*
C7A0.1032 (3)0.0363 (7)0.1227 (2)0.0385 (16)
C80.3060 (4)0.3439 (9)0.1745 (3)0.054 (2)
O80.3421 (3)0.4225 (6)0.1948 (2)0.0733 (18)
C90.1818 (4)0.3307 (8)0.1310 (3)0.0509 (19)
O90.1395 (3)0.4048 (6)0.1214 (2)0.0743 (17)
C100.2731 (3)0.2630 (6)0.0846 (3)0.0373 (16)
O100.2854 (3)0.2918 (5)0.04872 (17)0.0536 (13)
C110.2330 (3)0.1507 (8)0.2007 (2)0.0437 (17)
O110.2251 (3)0.1101 (6)0.23586 (18)0.0688 (17)
C120.2770 (4)0.3156 (8)0.0800 (3)0.0509 (19)
O120.3083 (3)0.4105 (6)0.0786 (2)0.0667 (16)
C130.1579 (4)0.2026 (7)0.0390 (3)0.0493 (19)
O130.1134 (3)0.2261 (6)0.0100 (2)0.0724 (17)
C140.1893 (4)0.2466 (8)0.1318 (3)0.058 (2)
O140.1675 (3)0.2969 (7)0.1611 (2)0.086 (2)
C150.2699 (3)0.0699 (7)0.0417 (2)0.0370 (16)
O150.2934 (2)0.0173 (5)0.01399 (16)0.0488 (13)
C220.3031 (4)0.1179 (7)0.1424 (2)0.0464 (18)
C230.3298 (4)0.1914 (8)0.1805 (3)0.0517 (19)
H23A0.32000.28270.18260.062*
C23A0.3749 (4)0.1237 (9)0.2186 (3)0.055 (2)
C240.4079 (4)0.1818 (11)0.2614 (3)0.075 (3)
H24A0.40540.27430.26680.090*
C250.4426 (5)0.1023 (14)0.2939 (3)0.082 (3)
H25A0.46600.14180.32150.098*
C260.4458 (4)0.0341 (13)0.2891 (3)0.076 (3)
H26A0.46860.08680.31370.092*
C270.4141 (4)0.0948 (10)0.2462 (3)0.068 (3)
H27A0.41670.18750.24140.082*
C27A0.3797 (3)0.0131 (9)0.2123 (2)0.050 (2)
C280.4003 (3)0.0694 (7)0.1163 (2)0.0362 (16)
C290.4252 (3)0.0438 (7)0.0980 (2)0.0445 (17)
H29A0.40800.12860.10260.053*
C300.4769 (4)0.0310 (8)0.0722 (3)0.053 (2)
H30A0.49320.10720.05910.063*
C310.5030 (3)0.0929 (8)0.0663 (3)0.050 (2)
H31A0.53700.10200.04910.060*
C320.4789 (3)0.2035 (7)0.0859 (3)0.0478 (18)
H32A0.49790.28760.08270.057*
C330.4267 (3)0.1943 (7)0.1107 (2)0.0455 (18)
H33A0.41020.27130.12310.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0404 (6)0.0398 (7)0.0376 (6)0.0022 (5)0.0138 (5)0.0051 (5)
Mn20.0427 (6)0.0358 (6)0.0420 (6)0.0031 (5)0.0102 (5)0.0014 (5)
P10.0371 (10)0.0366 (10)0.0351 (9)0.0027 (8)0.0099 (8)0.0024 (8)
P20.0394 (10)0.0433 (11)0.0350 (10)0.0038 (9)0.0074 (8)0.0001 (8)
C20.048 (5)0.047 (5)0.034 (4)0.001 (4)0.003 (3)0.006 (3)
C30.050 (5)0.039 (4)0.047 (4)0.003 (3)0.002 (4)0.004 (3)
C3A0.049 (5)0.032 (4)0.048 (4)0.004 (3)0.008 (4)0.005 (3)
C40.041 (5)0.038 (5)0.087 (6)0.002 (4)0.008 (4)0.003 (4)
C50.045 (5)0.050 (5)0.098 (7)0.008 (4)0.035 (5)0.001 (5)
C60.064 (6)0.057 (5)0.056 (5)0.016 (4)0.032 (4)0.007 (4)
C70.057 (5)0.047 (5)0.038 (4)0.011 (4)0.016 (3)0.004 (3)
C7A0.038 (4)0.033 (4)0.046 (4)0.004 (3)0.012 (3)0.007 (3)
C80.065 (5)0.053 (5)0.050 (5)0.010 (4)0.027 (4)0.006 (4)
O80.079 (4)0.064 (4)0.083 (4)0.025 (3)0.032 (3)0.033 (3)
C90.053 (5)0.043 (5)0.060 (5)0.003 (4)0.019 (4)0.008 (4)
O90.080 (4)0.062 (4)0.085 (4)0.020 (4)0.026 (4)0.007 (3)
C100.043 (4)0.019 (4)0.053 (4)0.003 (3)0.016 (3)0.002 (3)
O100.072 (4)0.043 (3)0.051 (3)0.000 (3)0.025 (3)0.010 (2)
C110.037 (4)0.057 (5)0.039 (4)0.000 (4)0.011 (3)0.008 (4)
O110.070 (4)0.100 (5)0.041 (3)0.008 (3)0.024 (3)0.002 (3)
C120.054 (5)0.038 (5)0.057 (5)0.003 (4)0.002 (4)0.004 (4)
O120.064 (4)0.045 (4)0.087 (4)0.015 (3)0.003 (3)0.008 (3)
C130.053 (5)0.030 (4)0.065 (5)0.002 (4)0.011 (4)0.007 (4)
O130.061 (4)0.073 (4)0.076 (4)0.017 (3)0.007 (3)0.004 (3)
C140.068 (5)0.045 (5)0.058 (5)0.011 (4)0.007 (4)0.004 (4)
O140.104 (5)0.080 (5)0.086 (4)0.012 (4)0.046 (4)0.036 (4)
C150.038 (4)0.034 (4)0.037 (4)0.003 (3)0.002 (3)0.012 (3)
O150.063 (3)0.048 (3)0.039 (3)0.007 (3)0.017 (2)0.004 (2)
C220.052 (5)0.047 (5)0.042 (4)0.011 (4)0.013 (4)0.000 (3)
C230.057 (5)0.042 (5)0.057 (5)0.006 (4)0.012 (4)0.010 (4)
C23A0.037 (4)0.071 (6)0.056 (5)0.000 (4)0.001 (4)0.017 (4)
C240.051 (5)0.113 (8)0.058 (6)0.007 (5)0.003 (4)0.031 (6)
C250.060 (6)0.141 (11)0.045 (6)0.002 (7)0.009 (5)0.025 (6)
C260.055 (5)0.138 (10)0.034 (5)0.003 (6)0.004 (4)0.017 (6)
C270.067 (6)0.092 (7)0.048 (5)0.010 (5)0.016 (4)0.019 (5)
C27A0.033 (4)0.081 (6)0.036 (4)0.006 (4)0.005 (3)0.001 (4)
C280.028 (4)0.046 (5)0.033 (4)0.000 (3)0.003 (3)0.002 (3)
C290.048 (4)0.040 (4)0.046 (4)0.010 (4)0.009 (3)0.006 (3)
C300.053 (5)0.049 (5)0.057 (5)0.010 (4)0.015 (4)0.004 (4)
C310.039 (4)0.058 (5)0.056 (5)0.011 (4)0.019 (4)0.009 (4)
C320.050 (4)0.037 (4)0.059 (5)0.013 (4)0.016 (4)0.002 (4)
C330.045 (4)0.046 (5)0.048 (4)0.002 (4)0.015 (3)0.003 (3)
Geometric parameters (Å, º) top
Mn1—C81.808 (9)C9—O91.135 (9)
Mn1—C91.824 (8)C10—O101.131 (7)
Mn1—C101.850 (7)C11—O111.116 (8)
Mn1—C111.872 (7)C12—O121.144 (8)
Mn1—P22.322 (2)C13—O131.144 (8)
Mn1—P12.401 (2)C14—O141.133 (9)
Mn2—C121.826 (8)C15—O151.126 (7)
Mn2—C131.846 (9)C22—C231.339 (10)
Mn2—C141.858 (9)C23—C23A1.458 (11)
Mn2—C151.875 (7)C23—H23A0.9300
Mn2—C222.056 (8)C23A—C27A1.370 (11)
Mn2—P12.382 (2)C23A—C241.408 (11)
P1—C21.823 (7)C24—C251.321 (13)
P1—C7A1.826 (6)C24—H24A0.9300
P2—C221.793 (8)C25—C261.359 (14)
P2—C27A1.855 (7)C25—H25A0.9300
P2—C281.862 (6)C26—C271.410 (12)
C2—C31.328 (9)C26—H26A0.9300
C2—H2A0.9300C27—C27A1.358 (10)
C3—C3A1.444 (9)C27—H27A0.9300
C3—H3A0.9300C28—C331.371 (9)
C3A—C7A1.406 (9)C28—C291.372 (9)
C3A—C41.413 (10)C29—C301.406 (9)
C4—C51.386 (10)C29—H29A0.9300
C4—H4A0.9300C30—C311.361 (10)
C5—C61.358 (11)C30—H30A0.9300
C5—H5A0.9300C31—C321.362 (10)
C6—C71.387 (10)C31—H31A0.9300
C6—H6A0.9300C32—C331.394 (9)
C7—C7A1.391 (9)C32—H32A0.9300
C7—H7A0.9300C33—H33A0.9300
C8—O81.157 (9)
C8—Mn1—C993.5 (4)C5—C6—H6A118.9
C8—Mn1—C1092.7 (3)C7—C6—H6A118.9
C9—Mn1—C1089.2 (3)C6—C7—C7A118.7 (7)
C8—Mn1—C1191.0 (3)C6—C7—H7A120.7
C9—Mn1—C1195.4 (3)C7A—C7—H7A120.7
C10—Mn1—C11174.0 (3)C7—C7A—C3A120.0 (6)
C8—Mn1—P293.8 (3)C7—C7A—P1129.8 (6)
C9—Mn1—P2172.6 (3)C3A—C7A—P1110.2 (5)
C10—Mn1—P289.2 (2)O8—C8—Mn1177.8 (7)
C11—Mn1—P285.8 (2)O9—C9—Mn1176.2 (7)
C8—Mn1—P1179.6 (2)O10—C10—Mn1179.3 (6)
C9—Mn1—P186.5 (2)O11—C11—Mn1176.3 (7)
C10—Mn1—P187.0 (2)O12—C12—Mn2176.5 (7)
C11—Mn1—P189.4 (2)O13—C13—Mn2179.4 (7)
P2—Mn1—P186.16 (7)O14—C14—Mn2177.0 (8)
C12—Mn2—C1397.7 (3)O15—C15—Mn2177.5 (6)
C12—Mn2—C1490.8 (3)C23—C22—P2107.8 (6)
C13—Mn2—C1490.9 (3)C23—C22—Mn2131.0 (6)
C12—Mn2—C1591.6 (3)P2—C22—Mn2120.6 (4)
C13—Mn2—C1590.9 (3)C22—C23—C23A117.9 (7)
C14—Mn2—C15176.7 (3)C22—C23—H23A121.0
C12—Mn2—C2285.1 (3)C23A—C23—H23A121.0
C13—Mn2—C22174.9 (3)C27A—C23A—C24118.7 (8)
C14—Mn2—C2284.8 (3)C27A—C23A—C23114.0 (7)
C15—Mn2—C2293.3 (3)C24—C23A—C23127.0 (8)
C12—Mn2—P1171.9 (2)C25—C24—C23A118.7 (10)
C13—Mn2—P190.3 (2)C25—C24—H24A120.6
C14—Mn2—P190.5 (2)C23A—C24—H24A120.6
C15—Mn2—P186.77 (19)C24—C25—C26123.4 (10)
C22—Mn2—P187.0 (2)C24—C25—H25A118.3
C2—P1—C7A89.1 (3)C26—C25—H25A118.3
C2—P1—Mn2110.2 (2)C25—C26—C27119.1 (9)
C7A—P1—Mn2115.6 (2)C25—C26—H26A120.5
C2—P1—Mn1109.5 (2)C27—C26—H26A120.5
C7A—P1—Mn1111.7 (2)C27A—C27—C26117.7 (9)
Mn2—P1—Mn1117.15 (8)C27A—C27—H27A121.2
C22—P2—C27A93.0 (4)C26—C27—H27A121.2
C22—P2—C28106.4 (3)C27—C27A—C23A122.3 (8)
C27A—P2—C28102.2 (3)C27—C27A—P2131.0 (7)
C22—P2—Mn1114.4 (2)C23A—C27A—P2106.7 (6)
C27A—P2—Mn1119.1 (3)C33—C28—C29120.4 (6)
C28—P2—Mn1118.1 (2)C33—C28—P2119.9 (5)
C3—C2—P1112.6 (5)C29—C28—P2119.7 (5)
C3—C2—H2A123.7C28—C29—C30119.8 (7)
P1—C2—H2A123.7C28—C29—H29A120.1
C2—C3—C3A114.9 (7)C30—C29—H29A120.1
C2—C3—H3A122.6C31—C30—C29120.1 (7)
C3A—C3—H3A122.6C31—C30—H30A120.0
C7A—C3A—C4119.7 (6)C29—C30—H30A120.0
C7A—C3A—C3113.2 (6)C30—C31—C32119.3 (6)
C4—C3A—C3127.1 (7)C30—C31—H31A120.4
C5—C4—C3A118.9 (7)C32—C31—H31A120.4
C5—C4—H4A120.6C31—C32—C33121.9 (7)
C3A—C4—H4A120.6C31—C32—H32A119.0
C6—C5—C4120.5 (7)C33—C32—H32A119.0
C6—C5—H5A119.7C28—C33—C32118.5 (7)
C4—C5—H5A119.7C28—C33—H33A120.7
C5—C6—C7122.2 (7)C32—C33—H33A120.7
 

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