Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100000408/qb0159sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100000408/qb0159Isup2.hkl |
CCDC reference: 142931
The title compound was prepared from (chloromethyl)ferrocene and [NEt4]2[Zn(dmio)2] and was recrystallized from dichloromethane/petroleum ether (333–353 K) producing orange crystals (m.p. 97–99°C).
The title compound crystallized in the monoclinic system; space group P21/n from the systematic absences. H atoms were treated as riding atoms with C—H distances in the range 0.93–0.97 Å.
Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); software used to prepare material for publication: SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).
[Fe2(C5H5)2(C15H12OS4)] | F(000) = 1184 |
Mr = 578.37 | Dx = 1.608 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 11.953 (2) Å | Cell parameters from 4915 reflections |
b = 18.433 (4) Å | θ = 2.0–28.3° |
c = 11.954 (2) Å | µ = 1.58 mm−1 |
β = 114.86 (3)° | T = 150 K |
V = 2389.8 (8) Å3 | Plate, orange |
Z = 4 | 0.40 × 0.35 × 0.10 mm |
KappaCCD diffractometer | 5785 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 2658 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.074 |
ϕ scans and ω scans with κ offsets | θmax = 28.3°, θmin = 2.0° |
Absorption correction: multi-scan SORTAV (Blessing, 1995, 1997) | h = −15→13 |
Tmin = 0.571, Tmax = 0.901 | k = −17→24 |
34055 measured reflections | l = −13→15 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.148 | H-atom parameters constrained |
S = 0.95 | w = 1/[σ2(Fo2) + (0.066P)2] where P = (Fo2 + 2Fc2)/3 |
5785 reflections | (Δ/σ)max = 0.004 |
289 parameters | Δρmax = 0.65 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
[Fe2(C5H5)2(C15H12OS4)] | V = 2389.8 (8) Å3 |
Mr = 578.37 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.953 (2) Å | µ = 1.58 mm−1 |
b = 18.433 (4) Å | T = 150 K |
c = 11.954 (2) Å | 0.40 × 0.35 × 0.10 mm |
β = 114.86 (3)° |
KappaCCD diffractometer | 5785 independent reflections |
Absorption correction: multi-scan SORTAV (Blessing, 1995, 1997) | 2658 reflections with I > 2σ(I) |
Tmin = 0.571, Tmax = 0.901 | Rint = 0.074 |
34055 measured reflections |
R[F2 > 2σ(F2)] = 0.056 | 0 restraints |
wR(F2) = 0.148 | H-atom parameters constrained |
S = 0.95 | Δρmax = 0.65 e Å−3 |
5785 reflections | Δρmin = −0.62 e Å−3 |
289 parameters |
Experimental. KappaCCD diffractometer using the following programs. COLLECT, Data collection software, Hooft (1999) [Hooft, R. (1998). Nonius BV, Delft, The Netherlands] is a graphical user interface written by Enraf–Nonius which encompasses the following programs. DENZO (Otwinowski & Minor, 1997) and indexing and data collection software package and a scaling package, SCALEPACK both of which programs are produced by the company HKL. Absorption corrections are performed by the SORTAVv package (Blessing, 1995, 1997) within the maXus suite of programs (Mackay et al., 1998) [Mackay, S., Gilmore, C·J., Edwards, C., Tremayne, M., Stewart, N. & Shankland, K. (1998). maXus. University of Glasgow, Scotland, UK]. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL97 input file. Low-temperature data is collected using an Oxford Cryosystems Cryostream Cooler (Cosier and Glazer, 1986) [Cosier, J. & Glazer, A·M. (1986). J. Appl. Cryst. 19, 105–107]. |
x | y | z | Uiso*/Ueq | ||
Fe1 | −0.29941 (6) | 0.25505 (4) | 0.29850 (6) | 0.0566 (2) | |
C6 | −0.2830 (4) | 0.1621 (2) | 0.2160 (4) | 0.0482 (11) | |
C7 | −0.2690 (4) | 0.2227 (3) | 0.1504 (4) | 0.0542 (12) | |
C8 | −0.1701 (4) | 0.2648 (3) | 0.2307 (5) | 0.0657 (14) | |
C9 | −0.1195 (4) | 0.2292 (3) | 0.3455 (5) | 0.0708 (15) | |
C10 | −0.1895 (4) | 0.1660 (3) | 0.3356 (4) | 0.0585 (12) | |
C11 | −0.4692 (6) | 0.2536 (4) | 0.3006 (8) | 0.096 (2) | |
C12 | −0.4609 (6) | 0.3118 (4) | 0.2347 (6) | 0.0880 (18) | |
C13 | −0.3666 (6) | 0.3554 (3) | 0.3102 (7) | 0.0832 (17) | |
C14 | −0.3106 (7) | 0.3232 (5) | 0.4270 (7) | 0.108 (2) | |
C15 | −0.3780 (8) | 0.2571 (4) | 0.4192 (7) | 0.101 (2) | |
Fe2 | 0.23686 (5) | 0.06832 (4) | 0.40033 (5) | 0.0491 (2) | |
C16 | 0.1729 (4) | 0.1307 (3) | 0.2453 (4) | 0.0553 (12) | |
C17 | 0.2296 (5) | 0.1742 (3) | 0.3495 (5) | 0.0689 (14) | |
C18 | 0.3518 (6) | 0.1513 (4) | 0.4123 (5) | 0.094 (2) | |
C19 | 0.3688 (5) | 0.0944 (4) | 0.3461 (6) | 0.098 (2) | |
C20 | 0.2593 (5) | 0.0818 (3) | 0.2415 (5) | 0.0683 (14) | |
C21 | 0.0953 (5) | 0.0268 (3) | 0.4331 (5) | 0.0770 (16) | |
C22 | 0.1827 (8) | 0.0588 (4) | 0.5383 (6) | 0.098 (2) | |
C23 | 0.2943 (7) | 0.0243 (4) | 0.5686 (5) | 0.104 (3) | |
C24 | 0.2746 (5) | −0.0309 (3) | 0.4820 (6) | 0.0824 (17) | |
C25 | 0.1506 (5) | −0.0271 (3) | 0.3990 (4) | 0.0676 (15) | |
S1 | −0.32007 (11) | 0.02516 (7) | 0.10942 (11) | 0.0612 (4) | |
S2 | −0.04135 (11) | 0.05923 (8) | 0.12090 (13) | 0.0760 (4) | |
S3 | −0.41854 (11) | 0.09068 (8) | −0.14281 (12) | 0.0713 (4) | |
S4 | −0.17445 (12) | 0.12700 (8) | −0.12924 (11) | 0.0683 (4) | |
O1 | −0.3823 (4) | 0.1598 (2) | −0.3176 (3) | 0.1018 (14) | |
C1 | −0.2911 (4) | 0.0664 (2) | −0.0068 (4) | 0.0479 (11) | |
C2 | −0.1799 (4) | 0.0839 (2) | −0.0020 (4) | 0.0508 (11) | |
C3 | −0.3355 (5) | 0.1317 (3) | −0.2179 (4) | 0.0704 (15) | |
C4 | −0.3770 (4) | 0.1034 (2) | 0.1645 (4) | 0.0588 (12) | |
C5 | 0.0426 (4) | 0.1425 (3) | 0.1518 (5) | 0.0841 (18) | |
H7 | −0.3173 | 0.2330 | 0.0678 | 0.065* | |
H8 | −0.1429 | 0.3084 | 0.2116 | 0.079* | |
H9 | −0.0520 | 0.2446 | 0.4154 | 0.085* | |
H10 | −0.1758 | 0.1324 | 0.3981 | 0.070* | |
H11 | −0.5277 | 0.2169 | 0.2703 | 0.115* | |
H12 | −0.5110 | 0.3205 | 0.1519 | 0.106* | |
H13 | −0.3436 | 0.3993 | 0.2877 | 0.100* | |
H14 | −0.2437 | 0.3408 | 0.4955 | 0.130* | |
H15 | −0.3629 | 0.2234 | 0.4818 | 0.122* | |
H17 | 0.1925 | 0.2119 | 0.3732 | 0.083* | |
H18 | 0.4106 | 0.1707 | 0.4851 | 0.113* | |
H19 | 0.4418 | 0.0686 | 0.3677 | 0.118* | |
H20 | 0.2468 | 0.0471 | 0.1809 | 0.082* | |
H21 | 0.0129 | 0.0402 | 0.3929 | 0.092* | |
H22 | 0.1687 | 0.0972 | 0.5813 | 0.117* | |
H23 | 0.3687 | 0.0357 | 0.6344 | 0.124* | |
H24 | 0.3328 | −0.0638 | 0.4801 | 0.099* | |
H25 | 0.1122 | −0.0570 | 0.3308 | 0.081* | |
H4A | −0.4490 | 0.1229 | 0.0968 | 0.071* | |
H4B | −0.4022 | 0.0874 | 0.2278 | 0.071* | |
H5A | 0.0430 | 0.1612 | 0.0762 | 0.101* | |
H5B | 0.0028 | 0.1780 | 0.1828 | 0.101* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0713 (4) | 0.0467 (5) | 0.0683 (5) | 0.0008 (3) | 0.0454 (4) | 0.0024 (3) |
C6 | 0.054 (2) | 0.048 (3) | 0.053 (3) | 0.006 (2) | 0.033 (2) | 0.005 (2) |
C7 | 0.057 (3) | 0.060 (3) | 0.053 (3) | 0.003 (2) | 0.031 (2) | 0.006 (2) |
C8 | 0.069 (3) | 0.059 (4) | 0.089 (4) | −0.008 (3) | 0.053 (3) | 0.002 (3) |
C9 | 0.054 (3) | 0.084 (4) | 0.070 (3) | −0.006 (3) | 0.022 (3) | −0.009 (3) |
C10 | 0.062 (3) | 0.057 (3) | 0.055 (3) | 0.008 (2) | 0.024 (2) | 0.011 (2) |
C11 | 0.112 (5) | 0.072 (5) | 0.149 (7) | 0.007 (4) | 0.100 (5) | 0.009 (5) |
C12 | 0.097 (4) | 0.072 (5) | 0.121 (5) | 0.024 (4) | 0.072 (4) | 0.005 (4) |
C13 | 0.106 (5) | 0.047 (4) | 0.129 (5) | 0.000 (3) | 0.081 (4) | −0.007 (4) |
C14 | 0.136 (6) | 0.114 (7) | 0.098 (5) | 0.007 (5) | 0.071 (5) | −0.039 (5) |
C15 | 0.171 (7) | 0.077 (5) | 0.110 (5) | 0.038 (5) | 0.111 (6) | 0.028 (4) |
Fe2 | 0.0452 (3) | 0.0511 (4) | 0.0468 (4) | −0.0096 (3) | 0.0153 (3) | 0.0054 (3) |
C16 | 0.048 (3) | 0.064 (3) | 0.053 (3) | −0.014 (2) | 0.020 (2) | 0.011 (2) |
C17 | 0.094 (4) | 0.042 (3) | 0.083 (3) | −0.011 (3) | 0.049 (3) | 0.004 (3) |
C18 | 0.078 (4) | 0.108 (6) | 0.071 (4) | −0.058 (4) | 0.007 (3) | 0.020 (4) |
C19 | 0.051 (3) | 0.129 (6) | 0.121 (6) | 0.011 (3) | 0.042 (4) | 0.057 (5) |
C20 | 0.076 (4) | 0.075 (4) | 0.066 (3) | −0.005 (3) | 0.042 (3) | 0.010 (3) |
C21 | 0.083 (4) | 0.079 (5) | 0.086 (4) | −0.007 (3) | 0.052 (4) | 0.023 (3) |
C22 | 0.172 (7) | 0.071 (5) | 0.082 (5) | −0.032 (5) | 0.086 (5) | −0.012 (4) |
C23 | 0.123 (6) | 0.100 (6) | 0.049 (3) | −0.053 (5) | −0.001 (4) | 0.023 (4) |
C24 | 0.079 (4) | 0.060 (4) | 0.102 (4) | 0.004 (3) | 0.031 (4) | 0.032 (3) |
C25 | 0.080 (4) | 0.059 (4) | 0.054 (3) | −0.027 (3) | 0.020 (3) | 0.005 (3) |
S1 | 0.0657 (7) | 0.0462 (8) | 0.0722 (8) | −0.0011 (6) | 0.0295 (6) | 0.0047 (6) |
S2 | 0.0508 (7) | 0.0678 (10) | 0.0803 (9) | −0.0024 (6) | −0.0010 (7) | 0.0228 (7) |
S3 | 0.0513 (7) | 0.0797 (10) | 0.0600 (8) | 0.0048 (6) | 0.0010 (6) | 0.0007 (7) |
S4 | 0.0711 (8) | 0.0751 (10) | 0.0585 (7) | 0.0049 (7) | 0.0271 (7) | 0.0099 (7) |
O1 | 0.118 (3) | 0.108 (4) | 0.049 (2) | 0.008 (3) | 0.006 (2) | 0.022 (2) |
C1 | 0.045 (2) | 0.049 (3) | 0.041 (2) | 0.003 (2) | 0.0104 (19) | −0.004 (2) |
C2 | 0.054 (3) | 0.049 (3) | 0.043 (2) | 0.002 (2) | 0.014 (2) | 0.000 (2) |
C3 | 0.081 (3) | 0.064 (4) | 0.046 (3) | 0.011 (3) | 0.008 (3) | −0.005 (2) |
C4 | 0.060 (3) | 0.053 (3) | 0.071 (3) | 0.006 (2) | 0.035 (2) | 0.006 (2) |
C5 | 0.067 (3) | 0.081 (4) | 0.081 (4) | −0.012 (3) | 0.009 (3) | 0.023 (3) |
Fe1—C15 | 2.026 (6) | Fe2—C25 | 2.035 (5) |
Fe1—C6 | 2.027 (4) | Fe2—C17 | 2.035 (5) |
Fe1—C14 | 2.032 (6) | Fe2—C16 | 2.037 (4) |
Fe1—C10 | 2.032 (5) | Fe2—C21 | 2.039 (5) |
Fe1—C8 | 2.032 (4) | Fe2—C20 | 2.041 (5) |
Fe1—C9 | 2.037 (5) | C16—C20 | 1.386 (7) |
Fe1—C7 | 2.040 (4) | C16—C17 | 1.395 (7) |
Fe1—C11 | 2.040 (6) | C16—C5 | 1.503 (6) |
Fe1—C12 | 2.041 (6) | C17—C18 | 1.398 (8) |
Fe1—C13 | 2.045 (5) | C18—C19 | 1.378 (9) |
C6—C10 | 1.397 (6) | C19—C20 | 1.399 (8) |
C6—C7 | 1.414 (6) | C21—C25 | 1.349 (7) |
C6—C4 | 1.494 (6) | C21—C22 | 1.384 (8) |
C7—C8 | 1.402 (6) | C22—C23 | 1.381 (9) |
C8—C9 | 1.407 (7) | C23—C24 | 1.400 (9) |
C9—C10 | 1.410 (7) | C24—C25 | 1.396 (7) |
C11—C12 | 1.359 (8) | S1—C1 | 1.742 (5) |
C11—C15 | 1.379 (9) | S1—C4 | 1.831 (5) |
C12—C13 | 1.370 (8) | S2—C2 | 1.750 (4) |
C13—C14 | 1.401 (8) | S2—C5 | 1.785 (5) |
C14—C15 | 1.441 (9) | S3—C1 | 1.756 (4) |
Fe2—C19 | 2.000 (6) | S3—C3 | 1.765 (6) |
Fe2—C23 | 2.004 (5) | S4—C2 | 1.741 (5) |
Fe2—C22 | 2.016 (6) | S4—C3 | 1.766 (5) |
Fe2—C18 | 2.020 (5) | O1—C3 | 1.200 (5) |
Fe2—C24 | 2.033 (5) | C1—C2 | 1.345 (6) |
C15—Fe1—C6 | 122.1 (2) | C22—Fe2—C24 | 67.2 (3) |
C15—Fe1—C14 | 41.6 (3) | C18—Fe2—C24 | 129.8 (3) |
C6—Fe1—C14 | 160.2 (3) | C19—Fe2—C25 | 132.2 (3) |
C15—Fe1—C10 | 108.1 (2) | C23—Fe2—C25 | 67.5 (2) |
C6—Fe1—C10 | 40.27 (17) | C22—Fe2—C25 | 66.2 (2) |
C14—Fe1—C10 | 125.2 (3) | C18—Fe2—C25 | 169.0 (3) |
C15—Fe1—C8 | 160.1 (3) | C24—Fe2—C25 | 40.1 (2) |
C6—Fe1—C8 | 68.63 (19) | C19—Fe2—C17 | 67.2 (3) |
C14—Fe1—C8 | 123.3 (3) | C23—Fe2—C17 | 129.9 (3) |
C10—Fe1—C8 | 68.2 (2) | C22—Fe2—C17 | 109.8 (2) |
C15—Fe1—C9 | 124.0 (3) | C18—Fe2—C17 | 40.3 (2) |
C6—Fe1—C9 | 68.24 (19) | C24—Fe2—C17 | 168.3 (2) |
C14—Fe1—C9 | 109.5 (3) | C25—Fe2—C17 | 150.3 (2) |
C10—Fe1—C9 | 40.55 (19) | C19—Fe2—C16 | 67.3 (2) |
C8—Fe1—C9 | 40.47 (19) | C23—Fe2—C16 | 168.8 (3) |
C15—Fe1—C7 | 158.2 (3) | C22—Fe2—C16 | 131.8 (3) |
C6—Fe1—C7 | 40.71 (16) | C18—Fe2—C16 | 67.8 (2) |
C14—Fe1—C7 | 158.3 (3) | C24—Fe2—C16 | 150.1 (2) |
C10—Fe1—C7 | 67.57 (18) | C25—Fe2—C16 | 119.03 (18) |
C8—Fe1—C7 | 40.29 (18) | C17—Fe2—C16 | 40.08 (19) |
C9—Fe1—C7 | 67.57 (19) | C19—Fe2—C21 | 169.6 (3) |
C15—Fe1—C11 | 39.6 (3) | C23—Fe2—C21 | 67.5 (2) |
C6—Fe1—C11 | 107.2 (2) | C22—Fe2—C21 | 39.9 (2) |
C14—Fe1—C11 | 67.4 (3) | C18—Fe2—C21 | 149.9 (3) |
C10—Fe1—C11 | 122.8 (2) | C24—Fe2—C21 | 66.7 (2) |
C8—Fe1—C11 | 158.9 (3) | C25—Fe2—C21 | 38.7 (2) |
C9—Fe1—C11 | 159.0 (3) | C17—Fe2—C21 | 118.8 (2) |
C7—Fe1—C11 | 123.2 (3) | C16—Fe2—C21 | 111.2 (2) |
C15—Fe1—C12 | 66.9 (3) | C19—Fe2—C20 | 40.5 (2) |
C6—Fe1—C12 | 121.4 (2) | C23—Fe2—C20 | 149.3 (3) |
C14—Fe1—C12 | 67.2 (3) | C22—Fe2—C20 | 169.8 (3) |
C10—Fe1—C12 | 156.8 (2) | C18—Fe2—C20 | 67.8 (2) |
C8—Fe1—C12 | 124.3 (2) | C24—Fe2—C20 | 117.8 (2) |
C9—Fe1—C12 | 161.1 (3) | C25—Fe2—C20 | 111.2 (2) |
C7—Fe1—C12 | 108.1 (2) | C17—Fe2—C20 | 67.2 (2) |
C11—Fe1—C12 | 38.9 (2) | C16—Fe2—C20 | 39.72 (19) |
C15—Fe1—C13 | 67.7 (2) | C21—Fe2—C20 | 131.9 (2) |
C6—Fe1—C13 | 156.8 (2) | C20—C16—C17 | 108.4 (4) |
C14—Fe1—C13 | 40.2 (2) | C20—C16—C5 | 128.6 (5) |
C10—Fe1—C13 | 162.3 (3) | C17—C16—C5 | 122.9 (5) |
C8—Fe1—C13 | 109.5 (2) | C20—C16—Fe2 | 70.3 (3) |
C9—Fe1—C13 | 126.3 (2) | C17—C16—Fe2 | 69.9 (3) |
C7—Fe1—C13 | 122.8 (2) | C5—C16—Fe2 | 129.3 (3) |
C11—Fe1—C13 | 65.7 (2) | C16—C17—C18 | 108.1 (5) |
C12—Fe1—C13 | 39.2 (2) | C16—C17—Fe2 | 70.0 (3) |
C10—C6—C7 | 107.3 (4) | C18—C17—Fe2 | 69.2 (3) |
C10—C6—C4 | 126.7 (4) | C19—C18—C17 | 107.2 (5) |
C7—C6—C4 | 126.0 (4) | C19—C18—Fe2 | 69.2 (3) |
C10—C6—Fe1 | 70.1 (3) | C17—C18—Fe2 | 70.4 (3) |
C7—C6—Fe1 | 70.1 (3) | C18—C19—C20 | 109.4 (5) |
C4—C6—Fe1 | 127.1 (3) | C18—C19—Fe2 | 70.7 (3) |
C8—C7—C6 | 108.6 (4) | C20—C19—Fe2 | 71.4 (3) |
C8—C7—Fe1 | 69.6 (3) | C16—C20—C19 | 107.0 (5) |
C6—C7—Fe1 | 69.1 (2) | C16—C20—Fe2 | 70.0 (3) |
C7—C8—C9 | 107.6 (4) | C19—C20—Fe2 | 68.2 (3) |
C7—C8—Fe1 | 70.1 (3) | C25—C21—C22 | 108.1 (6) |
C9—C8—Fe1 | 69.9 (3) | C25—C21—Fe2 | 70.5 (3) |
C8—C9—C10 | 107.9 (4) | C22—C21—Fe2 | 69.2 (3) |
C8—C9—Fe1 | 69.6 (3) | C23—C22—C21 | 108.6 (6) |
C10—C9—Fe1 | 69.5 (3) | C23—C22—Fe2 | 69.4 (4) |
C6—C10—C9 | 108.6 (4) | C21—C22—Fe2 | 70.9 (3) |
C6—C10—Fe1 | 69.7 (3) | C22—C23—C24 | 107.3 (5) |
C9—C10—Fe1 | 69.9 (3) | C22—C23—Fe2 | 70.4 (3) |
C12—C11—C15 | 109.9 (7) | C24—C23—Fe2 | 70.8 (3) |
C12—C11—Fe1 | 70.6 (3) | C25—C24—C23 | 106.7 (6) |
C15—C11—Fe1 | 69.6 (4) | C25—C24—Fe2 | 70.0 (3) |
C11—C12—C13 | 108.7 (6) | C23—C24—Fe2 | 68.6 (3) |
C11—C12—Fe1 | 70.5 (4) | C21—C25—C24 | 109.3 (5) |
C13—C12—Fe1 | 70.6 (3) | C21—C25—Fe2 | 70.8 (3) |
C12—C13—C14 | 108.9 (6) | C24—C25—Fe2 | 69.8 (3) |
C12—C13—Fe1 | 70.2 (3) | C1—S1—C4 | 99.9 (2) |
C14—C13—Fe1 | 69.4 (3) | C2—S2—C5 | 101.6 (2) |
C13—C14—C15 | 105.9 (6) | C1—S3—C3 | 97.2 (2) |
C13—C14—Fe1 | 70.4 (3) | C2—S4—C3 | 96.6 (2) |
C15—C14—Fe1 | 69.0 (3) | C2—C1—S1 | 126.5 (3) |
C11—C15—C14 | 106.5 (6) | C2—C1—S3 | 115.8 (3) |
C11—C15—Fe1 | 70.7 (3) | S1—C1—S3 | 117.6 (2) |
C14—C15—Fe1 | 69.4 (3) | C1—C2—S4 | 118.1 (3) |
C19—Fe2—C23 | 116.0 (3) | C1—C2—S2 | 122.9 (3) |
C19—Fe2—C22 | 148.6 (3) | S4—C2—S2 | 118.8 (3) |
C23—Fe2—C22 | 40.2 (3) | O1—C3—S3 | 124.2 (4) |
C19—Fe2—C18 | 40.1 (2) | O1—C3—S4 | 123.6 (5) |
C23—Fe2—C18 | 107.4 (2) | S3—C3—S4 | 112.2 (3) |
C22—Fe2—C18 | 116.8 (3) | C6—C4—S1 | 113.0 (3) |
C19—Fe2—C24 | 109.0 (3) | C16—C5—S2 | 110.3 (4) |
C23—Fe2—C24 | 40.6 (2) |
Experimental details
Crystal data | |
Chemical formula | [Fe2(C5H5)2(C15H12OS4)] |
Mr | 578.37 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 150 |
a, b, c (Å) | 11.953 (2), 18.433 (4), 11.954 (2) |
β (°) | 114.86 (3) |
V (Å3) | 2389.8 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.58 |
Crystal size (mm) | 0.40 × 0.35 × 0.10 |
Data collection | |
Diffractometer | KappaCCD diffractometer |
Absorption correction | Multi-scan SORTAV (Blessing, 1995, 1997) |
Tmin, Tmax | 0.571, 0.901 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 34055, 5785, 2658 |
Rint | 0.074 |
(sin θ/λ)max (Å−1) | 0.666 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.056, 0.148, 0.95 |
No. of reflections | 5785 |
No. of parameters | 289 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.65, −0.62 |
Computer programs: KappaCCD Server Software (Nonius, 1997), DENZO (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997b), SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).
Examination of the title structure, (I), with PLATON (Spek, 1998) showed that there were no solvent-accessible voids in the crystal lattice.