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The title compound, (μ-(SCH2)2CH2)Fe(CO)3Fe(CO)2P(C6H5)2NHCH2CH2CH3, has been prepared and characterized as a a model substance for a class of enzymes known as hydrogenases.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805010809/hb6172sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805010809/hb6172Isup2.hkl
Contains datablock I

CCDC reference: 271880

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.035
  • wR factor = 0.058
  • Data-to-parameter ratio = 20.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 47 Perc. PLAT230_ALERT_2_C Hirshfeld Test Diff for O3 - C3 .. 5.00 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - C5 .. 5.28 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe2 - C2 .. 5.36 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe2 - C3 .. 6.12 su PLAT420_ALERT_2_C D-H Without Acceptor N41 - H41 ... ?
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.22 From the CIF: _reflns_number_total 6253 Count of symmetry unique reflns 3690 Completeness (_total/calc) 169.46% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2563 Fraction of Friedel pairs measured 0.695 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 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 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: EXPOSE (Stoe, 1997); cell refinement: CELL (Stoe, 1997); data reduction: INTEGRATE (Stoe, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: PLATON (Spek, 2003).

Pentacarbonyl (diphenyl(N-propylamine)phosphine) diiron(µ-1,3-dithiolate propane) top
Crystal data top
[Fe2(C15H18NP)(C3H6S2)(CO)5]F(000) = 1232
Mr = 601.22Dx = 1.521 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 1371 reflections
a = 8.682 (1) Åθ = 1.9–28.1°
b = 9.421 (1) ŵ = 1.36 mm1
c = 32.108 (3) ÅT = 291 K
V = 2626.2 (5) Å3Plate, red
Z = 40.20 × 0.10 × 0.02 mm
Data collection top
STOE IPDS area-detector
diffractometer
6253 independent reflections
Radiation source: fine-focus sealed tube2923 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.099
Detector resolution: 6 pixels mm-1θmax = 28.2°, θmin = 2.3°
φ scansh = 1111
Absorption correction: numerical
(X-RED32; Stoe, 1997)
k = 1212
Tmin = 0.75, Tmax = 0.97l = 4242
27690 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.058 w = 1/[σ2(Fo2) + (0.01P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.89(Δ/σ)max = 0.001
6253 reflectionsΔρmax = 0.35 e Å3
311 parametersΔρmin = 0.84 e Å3
1 restraintAbsolute structure: Flack (1983); 2563 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.036 (15)
Special details top

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
Fe10.28788 (6)0.06254 (5)0.102001 (15)0.04155 (15)
Fe20.45970 (6)0.03675 (5)0.047010 (16)0.04245 (14)
S30.54619 (11)0.04152 (10)0.10978 (3)0.0463 (2)
S40.34847 (11)0.18106 (9)0.04295 (3)0.0454 (3)
P10.20254 (13)0.23396 (10)0.14276 (3)0.0433 (3)
C10.3218 (5)0.0943 (4)0.00993 (13)0.0508 (11)
O10.2305 (4)0.1284 (3)0.01376 (10)0.0888 (11)
C20.6234 (5)0.0339 (4)0.01329 (12)0.0535 (11)
O20.7258 (4)0.0377 (3)0.00926 (9)0.0868 (10)
C30.4738 (5)0.2098 (4)0.06717 (12)0.0509 (11)
O30.4795 (4)0.3237 (3)0.08086 (9)0.0792 (10)
C40.1111 (5)0.0248 (5)0.07886 (13)0.0579 (12)
O40.0068 (3)0.0036 (4)0.06261 (10)0.0946 (12)
C50.2696 (5)0.0750 (4)0.13867 (12)0.0496 (10)
O50.2610 (4)0.1667 (3)0.16256 (10)0.0860 (11)
C100.4863 (4)0.3226 (4)0.05054 (13)0.0569 (11)
H10A0.49560.37370.02440.068*
H10B0.44320.38820.07070.068*
C110.6436 (5)0.2850 (4)0.06459 (13)0.0613 (12)
H11A0.70310.37160.06720.074*
H11B0.69200.22770.04320.074*
C120.6522 (4)0.2060 (4)0.10492 (13)0.0523 (10)
H12A0.61710.26930.12680.063*
H12B0.75980.18550.11040.063*
C210.3480 (4)0.3322 (4)0.17160 (11)0.0425 (10)
C220.4319 (5)0.2651 (5)0.20313 (13)0.0646 (12)
H220.40900.17180.21020.078*
C230.5485 (6)0.3359 (6)0.22388 (15)0.0837 (15)
H230.60140.29150.24540.100*
C240.5857 (6)0.4722 (6)0.21241 (16)0.0812 (15)
H240.66590.51940.22570.097*
C250.5046 (5)0.5388 (5)0.18134 (15)0.0702 (13)
H250.52980.63130.17380.084*
C260.3867 (5)0.4700 (4)0.16127 (13)0.0510 (11)
H260.33210.51670.14040.061*
C310.0681 (5)0.1795 (4)0.18366 (12)0.0456 (10)
C320.0633 (6)0.2417 (4)0.22278 (14)0.0706 (13)
H320.13450.31170.22950.085*
C330.0452 (7)0.2014 (5)0.25185 (14)0.0820 (16)
H330.04590.24390.27800.098*
C340.1506 (6)0.1005 (5)0.24264 (17)0.0814 (17)
H340.22260.07300.26250.098*
C350.1508 (5)0.0396 (5)0.20427 (16)0.0700 (12)
H350.22450.02830.19760.084*
C360.0423 (5)0.0782 (4)0.17539 (12)0.0544 (11)
H360.04320.03470.14940.065*
N410.1078 (4)0.3581 (4)0.11635 (10)0.0550 (10)
H410.092 (5)0.347 (5)0.0931 (13)0.082*
C420.0071 (4)0.4658 (4)0.13413 (12)0.0557 (11)
H42A0.05340.50260.15940.067*
H42B0.09060.42270.14150.067*
C430.0209 (5)0.5858 (4)0.10458 (14)0.0683 (12)
H43A0.06160.54800.07870.082*
H43B0.07640.63180.09840.082*
C440.1312 (5)0.6940 (5)0.12140 (16)0.0906 (17)
H44A0.14500.76830.10130.136*
H44B0.09060.73340.14670.136*
H44C0.22860.64970.12700.136*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0483 (3)0.0383 (3)0.0380 (3)0.0003 (3)0.0030 (3)0.0003 (3)
Fe20.0522 (3)0.0371 (3)0.0380 (3)0.0017 (3)0.0051 (3)0.0015 (3)
S30.0525 (6)0.0447 (5)0.0416 (6)0.0002 (6)0.0044 (5)0.0010 (5)
S40.0549 (6)0.0407 (5)0.0407 (6)0.0014 (5)0.0037 (5)0.0041 (5)
P10.0525 (6)0.0396 (6)0.0380 (6)0.0057 (6)0.0044 (6)0.0041 (5)
C10.064 (3)0.045 (3)0.044 (3)0.006 (2)0.005 (2)0.002 (2)
O10.105 (3)0.084 (2)0.078 (2)0.021 (2)0.034 (2)0.0130 (19)
C20.070 (3)0.044 (2)0.046 (3)0.002 (3)0.005 (2)0.006 (2)
O20.086 (2)0.091 (2)0.083 (2)0.014 (2)0.046 (2)0.011 (2)
C30.057 (3)0.049 (2)0.047 (2)0.004 (2)0.009 (2)0.007 (2)
O30.121 (3)0.0411 (17)0.076 (2)0.0104 (19)0.0134 (19)0.0118 (16)
C40.055 (3)0.070 (3)0.049 (3)0.011 (3)0.012 (2)0.005 (2)
O40.060 (2)0.144 (3)0.080 (2)0.025 (2)0.0095 (18)0.002 (2)
C50.055 (3)0.043 (2)0.050 (2)0.011 (2)0.020 (2)0.005 (2)
O50.106 (3)0.0633 (19)0.089 (2)0.012 (2)0.032 (2)0.0331 (18)
C100.074 (3)0.039 (2)0.058 (3)0.011 (2)0.002 (3)0.007 (2)
C110.061 (3)0.060 (3)0.062 (3)0.021 (2)0.000 (2)0.004 (2)
C120.050 (2)0.054 (2)0.052 (3)0.007 (2)0.007 (2)0.003 (2)
C210.050 (3)0.040 (2)0.037 (2)0.009 (2)0.009 (2)0.0075 (19)
C220.079 (3)0.064 (3)0.050 (3)0.009 (3)0.004 (3)0.003 (2)
C230.080 (4)0.102 (4)0.069 (3)0.018 (4)0.016 (3)0.018 (3)
C240.067 (3)0.098 (4)0.079 (4)0.003 (4)0.003 (3)0.043 (3)
C250.066 (3)0.066 (3)0.079 (3)0.008 (3)0.018 (3)0.011 (3)
C260.057 (3)0.042 (2)0.055 (3)0.001 (2)0.006 (2)0.006 (2)
C310.051 (3)0.040 (2)0.046 (2)0.007 (2)0.005 (2)0.000 (2)
C320.087 (3)0.064 (3)0.060 (3)0.012 (3)0.018 (3)0.008 (3)
C330.106 (5)0.092 (4)0.048 (3)0.003 (4)0.026 (3)0.001 (3)
C340.081 (4)0.090 (4)0.073 (4)0.024 (3)0.032 (3)0.022 (3)
C350.064 (3)0.063 (3)0.083 (3)0.001 (3)0.017 (3)0.005 (3)
C360.053 (3)0.063 (3)0.047 (2)0.002 (3)0.011 (2)0.005 (2)
N410.070 (2)0.056 (2)0.039 (2)0.0246 (19)0.0012 (19)0.0058 (19)
C420.062 (3)0.052 (2)0.054 (2)0.015 (2)0.005 (2)0.002 (2)
C430.074 (3)0.049 (2)0.082 (3)0.005 (2)0.016 (3)0.011 (3)
C440.083 (4)0.074 (3)0.115 (4)0.020 (3)0.003 (3)0.009 (3)
Geometric parameters (Å, º) top
Fe1—C41.742 (5)C22—C231.383 (6)
Fe1—C51.758 (4)C22—H220.9300
Fe1—P12.2068 (11)C23—C241.375 (6)
Fe1—S42.2625 (11)C23—H230.9300
Fe1—S32.2652 (11)C24—C251.373 (6)
Fe1—Fe22.4936 (7)C24—H240.9300
Fe2—C31.758 (4)C25—C261.373 (5)
Fe2—C11.774 (5)C25—H250.9300
Fe2—C21.787 (4)C26—H260.9300
Fe2—S42.2716 (11)C31—C361.379 (5)
Fe2—S32.2735 (10)C31—C321.386 (5)
S3—C121.809 (3)C32—C331.380 (6)
S4—C101.808 (4)C32—H320.9300
P1—N411.662 (3)C33—C341.351 (6)
P1—C211.819 (4)C33—H330.9300
P1—C311.830 (4)C34—C351.359 (6)
C1—O11.145 (4)C34—H340.9300
C2—O21.147 (4)C35—C361.371 (5)
C3—O31.161 (4)C35—H350.9300
C4—O41.166 (4)C36—H360.9300
C5—O51.158 (4)N41—C421.456 (5)
C10—C111.482 (5)N41—H410.77 (4)
C10—H10A0.9700C42—C431.495 (5)
C10—H10B0.9700C42—H42A0.9700
C11—C121.495 (5)C42—H42B0.9700
C11—H11A0.9700C43—C441.500 (5)
C11—H11B0.9700C43—H43A0.9700
C12—H12A0.9700C43—H43B0.9700
C12—H12B0.9700C44—H44A0.9600
C21—C261.381 (5)C44—H44B0.9600
C21—C221.398 (5)C44—H44C0.9600
C4—Fe1—C593.2 (2)S3—C12—H12A107.7
C4—Fe1—P196.11 (14)C11—C12—H12B107.7
C5—Fe1—P196.43 (11)S3—C12—H12B107.7
C4—Fe1—S487.02 (14)H12A—C12—H12B107.1
C5—Fe1—S4161.09 (12)C26—C21—C22118.2 (4)
P1—Fe1—S4102.35 (4)C26—C21—P1121.6 (3)
C4—Fe1—S3154.36 (13)C22—C21—P1120.0 (3)
C5—Fe1—S387.19 (13)C23—C22—C21120.8 (4)
P1—Fe1—S3109.33 (4)C23—C22—H22119.6
S4—Fe1—S384.56 (4)C21—C22—H22119.6
C4—Fe1—Fe298.54 (13)C24—C23—C22119.6 (5)
C5—Fe1—Fe2104.57 (11)C24—C23—H23120.2
P1—Fe1—Fe2153.55 (4)C22—C23—H23120.2
S4—Fe1—Fe256.81 (3)C25—C24—C23120.1 (5)
S3—Fe1—Fe256.83 (3)C25—C24—H24120.0
C3—Fe2—C190.61 (18)C23—C24—H24120.0
C3—Fe2—C2100.48 (19)C24—C25—C26120.5 (5)
C1—Fe2—C297.75 (18)C24—C25—H25119.7
C3—Fe2—S4152.65 (13)C26—C25—H25119.7
C1—Fe2—S487.17 (12)C25—C26—C21120.8 (4)
C2—Fe2—S4106.83 (13)C25—C26—H26119.6
C3—Fe2—S387.21 (13)C21—C26—H26119.6
C1—Fe2—S3156.53 (13)C36—C31—C32116.5 (4)
C2—Fe2—S3105.63 (13)C36—C31—P1120.0 (3)
S4—Fe2—S384.17 (4)C32—C31—P1123.4 (3)
C3—Fe2—Fe197.39 (13)C33—C32—C31121.1 (4)
C1—Fe2—Fe1100.73 (12)C33—C32—H32119.4
C2—Fe2—Fe1154.05 (13)C31—C32—H32119.4
S4—Fe2—Fe156.46 (3)C34—C33—C32120.5 (5)
S3—Fe2—Fe156.51 (3)C34—C33—H33119.7
C12—S3—Fe1114.80 (13)C32—C33—H33119.7
C12—S3—Fe2111.68 (14)C33—C34—C35119.8 (5)
Fe1—S3—Fe266.65 (3)C33—C34—H34120.1
C10—S4—Fe1113.88 (14)C35—C34—H34120.1
C10—S4—Fe2112.17 (13)C34—C35—C36120.0 (4)
Fe1—S4—Fe266.73 (3)C34—C35—H35120.0
N41—P1—C21104.20 (18)C36—C35—H35120.0
N41—P1—C31104.33 (17)C35—C36—C31122.1 (4)
C21—P1—C31102.72 (18)C35—C36—H36119.0
N41—P1—Fe1112.24 (12)C31—C36—H36119.0
C21—P1—Fe1116.18 (12)C42—N41—P1126.0 (2)
C31—P1—Fe1115.75 (13)C42—N41—H41112 (4)
O1—C1—Fe2178.2 (4)P1—N41—H41120 (4)
O2—C2—Fe2176.7 (4)N41—C42—C43112.1 (3)
O3—C3—Fe2178.4 (4)N41—C42—H42A109.2
O4—C4—Fe1177.8 (5)C43—C42—H42A109.2
O5—C5—Fe1178.4 (4)N41—C42—H42B109.2
C11—C10—S4118.3 (3)C43—C42—H42B109.2
C11—C10—H10A107.7H42A—C42—H42B107.9
S4—C10—H10A107.7C42—C43—C44112.9 (4)
C11—C10—H10B107.7C42—C43—H43A109.0
S4—C10—H10B107.7C44—C43—H43A109.0
H10A—C10—H10B107.1C42—C43—H43B109.0
C10—C11—C12115.4 (3)C44—C43—H43B109.0
C10—C11—H11A108.4H43A—C43—H43B107.8
C12—C11—H11A108.4C43—C44—H44A109.5
C10—C11—H11B108.4C43—C44—H44B109.5
C12—C11—H11B108.4H44A—C44—H44B109.5
H11A—C11—H11B107.5C43—C44—H44C109.5
C11—C12—S3118.4 (3)H44A—C44—H44C109.5
C11—C12—H12A107.7H44B—C44—H44C109.5
 

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