Literature DB >> 22219779

μ(4)-Orthothio-carbonato-tetra-kis-[tri-carbonyl-iron(I)](2 Fe-Fe).

Yao-Cheng Shi, Huan-Ren Cheng, Li-Min Yuan, Qian-Kun Li.   

Abstract

The fused bis-butterfly-shaped title compound, [Fe(4)(CS(4))(CO)(12)], possesses an orthothio-carbonate (CS(4) (4-)) ligand that acts as a bridge between two Fe(2)(CO)(6) units. A short intra-molecular S⋯S contact [2.6984 (8) and 2.6977 (8) Å] occurs in each S(2)Fe(2)(CO)(6) fragment.

Entities:  

Year:  2011        PMID： 22219779      PMCID： PMC3246959          DOI： 10.1107/S1600536811041936

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For general background to related complexes, see: Mathur et al. (2009 ▶). For uses of R 3P/CS2 in coordination chemistry and organometallic chemistry, see: Galindo et al. (1999 ▶). For the synthesis of butterfly S2Fe2(CO)6 complexes, see: Song (2005 ▶). For related structures, see: Shaver et al. (1979 ▶); Ortega-Alfaro et al. (2004 ▶).

Experimental

Crystal data

[Fe4(CS4)(CO)12] M = 699.81 Triclinic, a = 9.0875 (9) Å b = 10.9002 (11) Å c = 12.6448 (13) Å α = 101.8859 (12)° β = 92.4964 (12)° γ = 110.0857 (12)° V = 1142.2 (2) Å3 Z = 2 Mo Kα radiation μ = 2.91 mm−1 T = 296 K 0.15 × 0.12 × 0.11 mm

Data collection

Bruker SMART APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T min = 0.658, T max = 0.721 10006 measured reflections 5128 independent reflections 4237 reflections with I > 2σ(I) R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.070 S = 1.04 5128 reflections 298 parameters 6 restraints Δρmax = 0.35 e Å−3 Δρmin = −0.27 e Å−3 Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT-Plus (Bruker, 2003 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SIR2004 (Burla et al., 2005 ▶); program(s) used to refine structure: SHELXTL (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶) and WinGX (Farrugia, 1999 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811041936/ng5239sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811041936/ng5239Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Fe4(CS4)(CO)12]Z = 2
Mr = 699.81F(000) = 684
Triclinic, P1Dx = 2.035 Mg m−3
a = 9.0875 (9) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.9002 (11) ÅCell parameters from 4237 reflections
c = 12.6448 (13) Åθ = 1.7–27.5°
α = 101.8859 (12)°µ = 2.91 mm−1
β = 92.4964 (12)°T = 296 K
γ = 110.0857 (12)°Prism, red
V = 1142.2 (2) Å30.15 × 0.12 × 0.11 mm
Bruker SMART APEX CCD diffractometer5128 independent reflections
Radiation source: fine-focus sealed tube4237 reflections with I > 2σ(I)
graphiteRint = 0.025
ω and φ scansθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)h = −11→11
Tmin = 0.658, Tmax = 0.721k = −14→14
10006 measured reflectionsl = −16→16
Refinement on F26 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.026Secondary atom site location: difference Fourier map
wR(F2) = 0.070w = 1/[σ2(Fo2) + (0.0332P)2] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
5128 reflectionsΔρmax = 0.35 e Å−3
298 parametersΔρmin = −0.27 e Å−3
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.
xyzUiso*/Ueq
C10.6561 (3)0.7935 (2)0.77984 (18)0.0440 (5)
C20.8526 (3)0.8863 (3)0.6347 (2)0.0506 (6)
C30.9578 (3)0.9654 (3)0.8400 (2)0.0495 (6)
C41.1219 (3)0.7705 (3)0.5832 (2)0.0576 (7)
C51.2260 (3)0.8567 (3)0.7869 (2)0.0499 (6)
C61.1533 (3)0.5863 (3)0.6883 (2)0.0520 (6)
C70.7715 (3)0.4656 (3)1.0044 (2)0.0518 (6)
C80.6869 (3)0.2015 (3)0.9062 (2)0.0571 (7)
C90.4644 (3)0.2955 (2)0.94124 (17)0.0461 (6)
C100.5449 (3)0.1072 (3)0.6532 (2)0.0533 (6)
C110.3306 (3)0.2117 (3)0.69401 (19)0.0538 (6)
C120.5320 (3)0.3000 (2)0.54991 (19)0.0461 (5)
C130.7801 (2)0.5349 (2)0.75626 (15)0.0326 (4)
Fe10.85275 (4)0.80727 (3)0.74597 (2)0.03532 (9)
Fe21.06610 (4)0.71578 (3)0.70503 (2)0.03858 (9)
Fe30.64765 (4)0.34558 (3)0.88425 (2)0.03604 (9)
Fe40.54035 (4)0.27424 (3)0.68685 (2)0.03649 (9)
O10.5347 (2)0.7883 (2)0.80095 (16)0.0652 (5)
O20.8523 (3)0.9343 (2)0.56303 (17)0.0808 (7)
O31.0252 (3)1.0659 (2)0.89976 (17)0.0801 (6)
O41.1562 (3)0.8060 (3)0.50561 (17)0.0906 (8)
O51.3234 (2)0.9495 (2)0.83931 (18)0.0764 (6)
O61.2101 (3)0.5078 (2)0.67522 (19)0.0802 (6)
O70.8437 (3)0.5364 (2)1.08183 (16)0.0849 (7)
O80.7108 (3)0.1096 (2)0.9194 (2)0.0923 (7)
O90.3472 (2)0.2622 (2)0.97500 (15)0.0716 (6)
O100.5481 (3)0.0019 (2)0.63331 (18)0.0840 (7)
O110.1982 (3)0.1726 (3)0.69931 (18)0.0901 (7)
O120.5245 (2)0.3122 (2)0.46352 (14)0.0717 (6)
S10.92568 (6)0.68363 (5)0.84778 (4)0.03454 (12)
S20.80928 (7)0.60300 (6)0.63482 (4)0.03789 (13)
S30.80213 (6)0.37272 (5)0.74843 (4)0.03674 (12)
S40.57807 (6)0.47963 (5)0.79267 (4)0.03420 (12)
U11U22U33U12U13U23
C10.0464 (14)0.0398 (13)0.0478 (12)0.0174 (11)0.0032 (10)0.0116 (10)
C20.0482 (15)0.0460 (14)0.0586 (14)0.0159 (12)0.0062 (12)0.0168 (12)
C30.0446 (14)0.0430 (14)0.0568 (14)0.0113 (12)0.0098 (11)0.0103 (12)
C40.0577 (17)0.0620 (17)0.0653 (17)0.0292 (14)0.0259 (14)0.0241 (14)
C50.0368 (14)0.0484 (15)0.0656 (16)0.0140 (12)0.0142 (12)0.0163 (13)
C60.0452 (15)0.0523 (15)0.0623 (15)0.0179 (12)0.0168 (12)0.0189 (13)
C70.0536 (16)0.0528 (15)0.0469 (13)0.0150 (13)0.0004 (11)0.0155 (12)
C80.0601 (17)0.0545 (16)0.0633 (16)0.0241 (14)0.0094 (13)0.0218 (13)
C90.0510 (15)0.0453 (14)0.0360 (11)0.0114 (12)0.0063 (10)0.0065 (10)
C100.0601 (17)0.0402 (14)0.0502 (14)0.0095 (12)0.0063 (12)0.0057 (11)
C110.0481 (16)0.0526 (16)0.0440 (13)0.0020 (13)0.0040 (11)0.0040 (11)
C120.0436 (14)0.0401 (13)0.0434 (13)0.0046 (11)0.0000 (10)0.0049 (10)
C130.0291 (11)0.0319 (10)0.0341 (10)0.0089 (9)0.0031 (8)0.0057 (8)
Fe10.03283 (18)0.03237 (17)0.03938 (17)0.00973 (13)0.00397 (13)0.00912 (13)
Fe20.03253 (18)0.03943 (18)0.04416 (18)0.01127 (14)0.01067 (13)0.01241 (14)
Fe30.03703 (18)0.03452 (17)0.03534 (16)0.01093 (14)0.00442 (13)0.00903 (13)
Fe40.03603 (18)0.03052 (17)0.03559 (16)0.00580 (13)0.00263 (13)0.00313 (13)
O10.0438 (11)0.0676 (13)0.0955 (14)0.0303 (10)0.0199 (10)0.0237 (11)
O20.0919 (17)0.0883 (16)0.0771 (13)0.0311 (14)0.0146 (12)0.0530 (13)
O30.0750 (15)0.0484 (12)0.0894 (15)0.0052 (11)0.0037 (12)−0.0119 (11)
O40.112 (2)0.112 (2)0.0796 (14)0.0537 (16)0.0579 (14)0.0566 (15)
O50.0456 (12)0.0589 (13)0.1025 (16)0.0024 (10)0.0007 (11)0.0014 (12)
O60.0805 (16)0.0736 (15)0.1125 (17)0.0495 (13)0.0371 (13)0.0347 (13)
O70.0857 (16)0.0882 (16)0.0530 (11)0.0075 (13)−0.0226 (11)0.0045 (11)
O80.1114 (19)0.0722 (15)0.1227 (19)0.0545 (15)0.0225 (15)0.0475 (15)
O90.0573 (13)0.0795 (15)0.0636 (12)0.0077 (11)0.0265 (10)0.0115 (11)
O100.1131 (19)0.0391 (11)0.0960 (16)0.0283 (12)0.0166 (14)0.0056 (11)
O110.0473 (13)0.1058 (19)0.0861 (15)−0.0053 (12)0.0126 (11)0.0119 (14)
O120.0788 (14)0.0732 (14)0.0428 (10)0.0033 (11)−0.0061 (9)0.0147 (9)
S10.0314 (3)0.0334 (3)0.0332 (2)0.0058 (2)0.0010 (2)0.0063 (2)
S20.0398 (3)0.0375 (3)0.0317 (3)0.0086 (2)0.0031 (2)0.0077 (2)
S30.0338 (3)0.0338 (3)0.0430 (3)0.0135 (2)0.0070 (2)0.0071 (2)
S40.0298 (3)0.0309 (3)0.0400 (3)0.0097 (2)0.0045 (2)0.0062 (2)
C1—O11.131 (3)C10—Fe41.798 (3)
C1—Fe11.819 (3)C11—O111.140 (3)
C2—O21.136 (3)C11—Fe41.804 (3)
C2—Fe11.795 (2)C12—O121.129 (3)
C3—O31.142 (3)C12—Fe41.813 (2)
C3—Fe11.796 (3)C13—S11.827 (2)
C4—O41.145 (3)C13—S21.8300 (19)
C4—Fe21.795 (3)C13—S31.830 (2)
C5—O51.142 (3)C13—S41.837 (2)
C5—Fe21.795 (3)Fe1—S12.2730 (6)
C6—O61.130 (3)Fe1—S22.2688 (7)
C6—Fe21.824 (3)Fe1—Fe22.4949 (5)
C7—O71.127 (3)Fe2—S12.2723 (6)
C7—Fe31.818 (3)Fe2—S22.2685 (7)
C8—O81.138 (3)Fe3—S32.2676 (6)
C8—Fe31.796 (3)Fe3—S42.2680 (6)
C9—O91.134 (3)Fe3—Fe42.5007 (5)
C9—Fe31.798 (3)Fe4—S32.2712 (7)
C10—O101.135 (3)Fe4—S42.2626 (6)
S1···S22.6984 (8)S3···S42.6977 (8)
O1—C1—Fe1178.3 (2)C6—Fe2—Fe1154.51 (8)
O2—C2—Fe1178.8 (2)S2—Fe2—Fe156.649 (18)
O3—C3—Fe1179.6 (3)S1—Fe2—Fe156.723 (17)
O4—C4—Fe2179.2 (3)C8—Fe3—C991.66 (12)
O5—C5—Fe2177.0 (2)C8—Fe3—C797.13 (12)
O6—C6—Fe2177.6 (2)C9—Fe3—C798.48 (11)
O7—C7—Fe3176.7 (2)C8—Fe3—S393.97 (9)
O8—C8—Fe3179.5 (3)C9—Fe3—S3155.51 (7)
O9—C9—Fe3178.5 (2)C7—Fe3—S3104.42 (8)
O10—C10—Fe4179.2 (3)C8—Fe3—S4158.63 (9)
O11—C11—Fe4179.5 (3)C9—Fe3—S493.86 (8)
O12—C12—Fe4178.0 (2)C7—Fe3—S4102.43 (8)
S1—C13—S3118.10 (10)S3—Fe3—S472.99 (2)
S1—C13—S295.10 (10)C8—Fe3—Fe4102.35 (9)
S3—C13—S2117.13 (11)C9—Fe3—Fe498.88 (7)
S1—C13—S4116.95 (11)C7—Fe3—Fe4153.39 (8)
S3—C13—S494.73 (9)S3—Fe3—Fe456.635 (18)
S2—C13—S4116.62 (10)S4—Fe3—Fe456.394 (17)
C2—Fe1—C392.20 (12)C10—Fe4—C1192.11 (13)
C2—Fe1—C197.54 (11)C10—Fe4—C1297.98 (11)
C3—Fe1—C196.81 (11)C11—Fe4—C1297.54 (11)
C2—Fe1—S293.44 (9)C10—Fe4—S4157.10 (8)
C3—Fe1—S2158.89 (8)C11—Fe4—S493.60 (9)
C1—Fe1—S2102.58 (8)C12—Fe4—S4103.21 (8)
C2—Fe1—S1156.74 (8)C10—Fe4—S394.03 (9)
C3—Fe1—S194.58 (8)C11—Fe4—S3157.73 (8)
C1—Fe1—S1103.69 (7)C12—Fe4—S3102.76 (8)
S2—Fe1—S172.90 (2)S4—Fe4—S373.03 (2)
C2—Fe1—Fe2100.11 (8)C10—Fe4—Fe3100.52 (8)
C3—Fe1—Fe2102.33 (8)C11—Fe4—Fe3101.33 (8)
C1—Fe1—Fe2153.30 (7)C12—Fe4—Fe3152.93 (8)
S2—Fe1—Fe256.636 (18)S4—Fe4—Fe356.600 (16)
S1—Fe1—Fe256.695 (17)S3—Fe4—Fe356.499 (16)
C5—Fe2—C491.26 (13)C13—S1—Fe288.02 (6)
C5—Fe2—C6100.64 (12)C13—S1—Fe187.12 (6)
C4—Fe2—C696.91 (11)Fe2—S1—Fe166.582 (18)
C5—Fe2—S2153.65 (8)C13—S2—Fe288.06 (7)
C4—Fe2—S293.88 (9)C13—S2—Fe187.17 (7)
C6—Fe2—S2104.35 (9)Fe2—S2—Fe166.715 (19)
C5—Fe2—S193.23 (8)C13—S3—Fe387.77 (7)
C4—Fe2—S1157.61 (9)C13—S3—Fe487.52 (7)
C6—Fe2—S1103.77 (8)Fe3—S3—Fe466.867 (19)
S2—Fe2—S172.92 (2)C13—S4—Fe487.60 (7)
C5—Fe2—Fe197.00 (8)C13—S4—Fe387.58 (6)
C4—Fe2—Fe1100.96 (8)Fe4—S4—Fe367.006 (19)
C13—S11.827 (2)
C13—S21.8300 (19)
C13—S31.830 (2)
C13—S41.837 (2)
Fe1—S12.2730 (6)
Fe1—S22.2688 (7)
Fe1—Fe22.4949 (5)
Fe2—S12.2723 (6)
Fe2—S22.2685 (7)
Fe3—S32.2676 (6)
Fe3—S42.2680 (6)
Fe3—Fe42.5007 (5)
Fe4—S32.2712 (7)
Fe4—S42.2626 (6)
S1—C13—S295.10 (10)
S3—C13—S494.73 (9)
  3 in total

1.  Investigations on butterfly Fe/S cluster S-centered anions (mu-S-)2Fe2(CO)6, (mu-S-)(mu-RS)Fe2(CO)6, and related species.

Authors:  Li-Cheng Song
Journal:  Acc Chem Res       Date:  2005-01       Impact factor: 22.384

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  3 in total
  3 in total

1.  Rational Synthesis of the Carbonyl(perthiolato)diiron [Fe2(S3CPh2)(CO)6] and Related Complexes.

Authors:  Peihua Zhao; Danielle L Gray; Thomas B Rauchfuss
Journal:  Eur J Inorg Chem       Date:  2016-05-19       Impact factor: 2.524

Review 2.  Synthesis of Diiron(I) Dithiolato Carbonyl Complexes.

Authors:  Yulong Li; Thomas B Rauchfuss
Journal:  Chem Rev       Date:  2016-06-03       Impact factor: 60.622

3.  Crystal structure of [μ2-3,3-dimethyl-4-(propan-2-yl-idene)thietane-2,2-dithiol-ato-κ(4) S:S':S:S']bis[tricarbonyl-iron(I)](Fe-Fe).

Authors:  Peihua Zhao; Jeffery A Bertke; Thomas B Rauchfuss
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2015-10-10
  3 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.