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In the crystal structure of the title compound, [Fe2(C12H10P)2(CO)6]·CH2Cl2, the complex mol­ecule lies across a mirror plane. Two diphosphide ligands bridge two (CO)3Fe fragments to form a dinuclear complex, in which the Fe—Fe distance is 2.6701 (6) Å. Two aromatic rings within the same molecule inter­act by face-to-face π–π stacking, with a centroid-to-centroid distance of 3.601 (2) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020982/xu6018sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020982/xu6018Isup2.hkl
Contains datablock I

CCDC reference: 282703

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.044
  • wR factor = 0.132
  • Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.71 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe - C10 .. 7.17 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe - C11 .. 6.10 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe - C12 .. 6.66 su PLAT331_ALERT_2_C Small Average Phenyl C-C Dist. C21 -C22_b 1.37 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXL97 and WinGX2003 (Farrugia, 1999).

Di-µ-diphenylphosphido-bis[tricarbonyliron(II)] dichloromethane solvate top
Crystal data top
[Fe2(C12H10P)2(CO)6]·CH2Cl2F(000) = 744
Mr = 735.03Dx = 1.494 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 600 reflections
a = 11.3218 (11) Åθ = 20–25°
b = 12.7214 (13) ŵ = 1.19 mm1
c = 11.8011 (12) ÅT = 293 K
β = 105.976 (2)°Rectangular, yellow
V = 1634.1 (3) Å30.22 × 0.12 × 0.09 mm
Z = 2
Data collection top
Bruker SMART area-detector
diffractometer
Rint = 0.022
Graphite monochromatorθmax = 27.5°, θmin = 1.8°
φ and ω scansh = 1412
8071 measured reflectionsk = 1516
3826 independent reflectionsl = 715
2896 reflections with I > 2σ(I)
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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.132H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0878P)2]
where P = (Fo2 + 2Fc2)/3
3826 reflections(Δ/σ)max < 0.001
211 parametersΔρmax = 1.17 e Å3
0 restraintsΔρmin = 0.76 e Å3
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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
Fe0.39139 (3)0.14753 (3)0.29892 (3)0.0335 (1)
P10.25204 (8)0.250000.34476 (8)0.0341 (3)
P20.34056 (8)0.250000.14062 (8)0.0323 (3)
O100.2581 (2)0.04789 (18)0.2297 (2)0.0665 (8)
O110.6258 (2)0.0945 (2)0.2550 (3)0.0899 (11)
O120.5111 (3)0.1175 (2)0.5507 (2)0.0752 (9)
C10.2380 (4)0.250000.4948 (3)0.0484 (14)
C20.2306 (4)0.1567 (3)0.5520 (3)0.0693 (14)
C30.2154 (5)0.1576 (4)0.6652 (4)0.099 (2)
C40.2076 (6)0.250000.7189 (5)0.102 (3)
C50.0890 (3)0.250000.2656 (3)0.0450 (14)
C60.0254 (3)0.1580 (3)0.2403 (4)0.0751 (13)
C70.1013 (3)0.1586 (4)0.1867 (4)0.098 (2)
C80.1627 (5)0.250000.1596 (5)0.090 (3)
C100.3093 (2)0.0285 (2)0.2564 (2)0.0427 (9)
C110.5349 (3)0.1158 (3)0.2707 (3)0.0518 (10)
C120.4628 (3)0.1281 (2)0.4536 (3)0.0489 (10)
C210.4315 (3)0.250000.0335 (3)0.0384 (11)
C220.4609 (3)0.1578 (2)0.0120 (3)0.0592 (11)
C230.5231 (4)0.1586 (3)0.0980 (3)0.0741 (16)
C240.5535 (5)0.250000.1395 (4)0.0722 (19)
C250.1870 (3)0.250000.0380 (3)0.0379 (11)
C260.1306 (3)0.1576 (3)0.0043 (3)0.0626 (12)
C270.0153 (4)0.1579 (3)0.0865 (3)0.0823 (16)
C280.0408 (5)0.250000.1272 (5)0.080 (2)
Cl10.8433 (4)0.1424 (3)0.5360 (3)0.379 (3)
C300.8992 (9)0.250000.4969 (9)0.131 (4)
H20.235700.093070.514910.0831*
H30.210600.094580.703690.1184*
H40.196620.250000.794140.1233*
H60.066600.094330.258830.0899*
H70.143490.095240.169630.1174*
H80.246550.250000.122480.1081*
H220.439020.094030.015030.0708*
H230.543890.095380.127160.0888*
H240.595580.250000.196980.0865*
H260.169210.094100.021800.0757*
H270.023260.094620.113590.0989*
H280.117190.250000.182600.0962*
H30A0.883610.250000.411820.1577*
H30B0.987580.250000.530920.1577*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.0317 (2)0.0326 (2)0.0339 (2)0.0018 (1)0.0050 (2)0.0019 (1)
P10.0353 (5)0.0381 (5)0.0294 (5)0.00000.0095 (4)0.0000
P20.0316 (4)0.0346 (5)0.0307 (5)0.00000.0087 (4)0.0000
O100.0616 (13)0.0476 (13)0.0855 (17)0.0158 (11)0.0121 (12)0.0098 (12)
O110.0485 (14)0.112 (2)0.115 (2)0.0262 (15)0.0321 (14)0.0180 (19)
O120.0931 (18)0.0703 (15)0.0438 (13)0.0202 (13)0.0123 (12)0.0066 (11)
C10.041 (2)0.071 (3)0.034 (2)0.00000.0115 (16)0.0000
C20.078 (2)0.080 (3)0.056 (2)0.0022 (18)0.0287 (19)0.0151 (17)
C30.102 (3)0.143 (5)0.059 (3)0.011 (3)0.036 (2)0.039 (3)
C40.087 (4)0.190 (8)0.037 (3)0.00000.028 (3)0.0000
C50.037 (2)0.067 (3)0.033 (2)0.00000.0131 (16)0.0000
C60.0424 (18)0.077 (2)0.105 (3)0.0072 (16)0.0188 (19)0.029 (2)
C70.043 (2)0.139 (4)0.111 (4)0.023 (2)0.019 (2)0.053 (3)
C80.038 (3)0.153 (7)0.079 (4)0.00000.015 (3)0.0000
C100.0404 (14)0.0436 (16)0.0431 (15)0.0025 (12)0.0097 (12)0.0001 (12)
C110.0412 (16)0.0553 (17)0.0564 (19)0.0055 (14)0.0092 (14)0.0050 (15)
C120.0536 (18)0.0389 (15)0.0474 (18)0.0071 (12)0.0027 (14)0.0022 (13)
C210.0370 (19)0.042 (2)0.037 (2)0.00000.0115 (15)0.0000
C220.072 (2)0.0488 (18)0.067 (2)0.0043 (15)0.0362 (19)0.0068 (14)
C230.098 (3)0.067 (2)0.077 (3)0.0095 (19)0.057 (2)0.0096 (18)
C240.077 (3)0.094 (4)0.061 (3)0.00000.045 (3)0.0000
C250.0353 (18)0.055 (2)0.0242 (17)0.00000.0093 (14)0.0000
C260.057 (2)0.064 (2)0.054 (2)0.0153 (15)0.0064 (16)0.0037 (15)
C270.059 (2)0.104 (3)0.068 (3)0.029 (2)0.0092 (19)0.000 (2)
C280.045 (3)0.129 (5)0.055 (3)0.00000.006 (2)0.0000
Cl10.421 (5)0.487 (6)0.176 (2)0.355 (5)0.008 (3)0.052 (3)
C300.133 (6)0.121 (6)0.170 (8)0.00000.093 (6)0.0000
Geometric parameters (Å, º) top
Fe—P12.2250 (9)C21—C221.369 (3)
Fe—P22.2200 (8)C21—C22i1.369 (3)
Fe—C101.775 (3)C22—C231.385 (5)
Fe—C111.792 (4)C23—C241.343 (5)
Fe—C121.798 (3)C25—C261.365 (4)
Fe—Fei2.6071 (6)C25—C26i1.365 (4)
Cl1—C301.627 (7)C26—C271.396 (5)
P1—C11.821 (4)C27—C281.356 (5)
P1—C51.825 (4)C2—H20.9295
P2—C211.837 (4)C3—H30.9304
P2—C251.825 (4)C4—H40.9298
O10—C101.131 (3)C6—H60.9302
O11—C111.128 (4)C7—H70.9303
O12—C121.134 (4)C8—H80.9296
C1—C2i1.379 (4)C22—H220.9299
C1—C21.379 (4)C23—H230.9302
C2—C31.393 (6)C24—H240.9301
C3—C41.350 (6)C26—H260.9297
C5—C61.363 (4)C27—H270.9295
C5—C6i1.363 (4)C28—H280.9296
C6—C71.399 (5)C30—H30A0.9704
C7—C81.347 (6)C30—H30B0.9702
P1—Fe—P279.84 (3)P2—C21—C22120.86 (19)
P1—Fe—C10102.55 (8)P2—C21—C22i120.86 (19)
P1—Fe—C11156.48 (12)C22—C21—C22i118.0 (3)
P1—Fe—C1289.11 (11)C21—C22—C23120.6 (3)
Fei—Fe—P154.14 (2)C22—C23—C24120.4 (4)
P2—Fe—C10105.59 (8)C23—C24—C23i120.0 (5)
P2—Fe—C1190.81 (12)P2—C25—C26120.5 (2)
P2—Fe—C12151.02 (9)P2—C25—C26i120.5 (2)
Fei—Fe—P254.04 (2)C26—C25—C26i118.9 (3)
C10—Fe—C11100.73 (14)C25—C26—C27120.4 (3)
C10—Fe—C12102.93 (12)C26—C27—C28120.4 (4)
Fei—Fe—C10148.53 (8)C27—C28—C27i119.5 (5)
C11—Fe—C1288.87 (16)C1—C2—H2119.93
Fei—Fe—C11103.02 (12)C3—C2—H2119.92
Fei—Fe—C1297.90 (8)C2—C3—H3120.02
Fe—P1—C1119.60 (11)C4—C3—H3120.07
Fe—P1—C5124.09 (8)C3—C4—H4119.44
Fe—P1—Fei71.73 (3)C3i—C4—H4119.44
C1—P1—C598.69 (18)C5—C6—H6119.70
Fei—P1—C1119.60 (11)C7—C6—H6119.76
Fei—P1—C5124.09 (8)C6—C7—H7119.64
Fe—P2—C21120.96 (9)C8—C7—H7119.72
Fe—P2—C25122.51 (9)C7—C8—H8120.34
Fe—P2—Fei71.91 (3)C7i—C8—H8120.34
C21—P2—C2598.94 (16)C21—C22—H22119.77
Fei—P2—C21120.96 (9)C23—C22—H22119.66
Fei—P2—C25122.51 (9)C22—C23—H23119.74
P1—C1—C2120.6 (2)C24—C23—H23119.83
P1—C1—C2i120.6 (2)C23—C24—H24120.01
C2—C1—C2i118.7 (3)C23i—C24—H24120.01
C1—C2—C3120.2 (4)C25—C26—H26119.81
C2—C3—C4119.9 (5)C27—C26—H26119.81
C3—C4—C3i121.1 (5)C26—C27—H27119.84
P1—C5—C6120.7 (2)C28—C27—H27119.77
P1—C5—C6i120.7 (2)C27—C28—H28120.23
C6—C5—C6i118.3 (3)C27i—C28—H28120.23
C5—C6—C7120.5 (4)Cl1—C30—Cl1i114.5 (7)
C6—C7—C8120.6 (4)Cl1—C30—H30A108.62
C7—C8—C7i119.3 (5)Cl1—C30—H30B108.66
Fe—C10—O10179.3 (2)H30A—C30—H30B107.54
Fe—C11—O11178.5 (3)Cl1i—C30—H30A108.62
Fe—C12—O12177.8 (3)Cl1i—C30—H30B108.66
P1—Fe—Fei—P2104.81 (4)C12—Fe—P2—C25133.9 (2)
P2—Fe—Fei—P1104.81 (4)Fei—Fe—P2—C25117.53 (10)
C10—Fe—Fei—P148.13 (15)P1—Fe—P2—Fei52.75 (3)
C10—Fe—Fei—P256.68 (15)C10—Fe—P2—Fei153.07 (8)
C10—Fe—Fei—C10i0.0 (2)C11—Fe—P2—Fei105.55 (12)
C10—Fe—Fei—C11i138.07 (18)C12—Fe—P2—Fei16.4 (2)
C10—Fe—Fei—C12i131.26 (19)P1—Fei—P2—Fe52.75 (3)
C11—Fe—Fei—P1173.80 (12)Fe—Fei—P2—C21115.80 (10)
C11—Fe—Fei—P281.39 (12)Fe—Fei—P2—C25117.53 (10)
C11—Fe—Fei—C10i138.07 (18)Fe—P1—C1—C248.7 (4)
C11—Fe—Fei—C11i0.00 (16)C5—P1—C1—C289.0 (4)
C11—Fe—Fei—C12i90.67 (16)Fei—P1—C1—C2133.4 (3)
C12—Fe—Fei—P183.13 (12)Fe—P1—C1—C2i133.4 (3)
C12—Fe—Fei—P2172.06 (12)Fe—P1—C5—C6i138.2 (3)
C12—Fe—Fei—C10i131.26 (19)Fe—P1—C5—C648.1 (4)
C12—Fe—Fei—C11i90.67 (16)C1—P1—C5—C686.9 (3)
C12—Fe—Fei—C12i0.00 (16)Fei—P1—C5—C6138.2 (3)
P2—Fe—P1—C1166.91 (12)Fe—P2—C25—C26i136.6 (3)
C10—Fe—P1—C189.22 (14)Fei—P2—C25—C26136.6 (3)
C11—Fe—P1—C199.0 (3)Fe—P2—C21—C2250.2 (3)
C12—Fe—P1—C113.83 (15)Fe—P2—C21—C22i136.6 (3)
Fei—Fe—P1—C1114.25 (12)Fei—P2—C21—C22136.6 (3)
P2—Fe—P1—C566.63 (10)C21—P2—C25—C2687.6 (3)
C10—Fe—P1—C537.24 (13)C25—P2—C21—C2286.6 (3)
C11—Fe—P1—C5134.6 (3)Fe—P2—C25—C2648.3 (3)
C12—Fe—P1—C5140.29 (14)C2i—C1—C2—C30.3 (7)
Fei—Fe—P1—C5119.29 (11)P1—C1—C2—C3177.7 (4)
P2—Fe—P1—Fei52.66 (3)C1—C2—C3—C40.2 (8)
C10—Fe—P1—Fei156.53 (8)C2—C3—C4—C3i0.6 (9)
C11—Fe—P1—Fei15.3 (3)P1—C5—C6—C7175.7 (3)
C12—Fe—P1—Fei100.42 (10)C6i—C5—C6—C71.8 (6)
P2—Fei—P1—Fe52.66 (3)C5—C6—C7—C80.3 (7)
Fe—Fei—P1—C1114.25 (12)C6—C7—C8—C7i1.3 (8)
Fe—Fei—P1—C5119.29 (11)C22i—C21—C22—C232.6 (5)
P1—Fe—P2—C21168.55 (10)P2—C21—C22—C23176.1 (3)
C10—Fe—P2—C2191.13 (12)C21—C22—C23—C241.2 (6)
C11—Fe—P2—C2110.26 (15)C22—C23—C24—C23i0.3 (7)
C12—Fe—P2—C2199.4 (3)P2—C25—C26—C27177.3 (3)
Fei—Fe—P2—C21115.80 (10)C26i—C25—C26—C272.1 (5)
P1—Fe—P2—C2564.78 (10)C25—C26—C27—C281.4 (6)
C10—Fe—P2—C2535.54 (13)C26—C27—C28—C27i0.7 (7)
C11—Fe—P2—C25136.92 (15)
Symmetry code: (i) x, y+1/2, z.
 

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