Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010200330X/jz1495sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827010200330X/jz1495Isup2.hkl |
CCDC reference: 184470
Data collection: IPDS (Stoe & Cie, 1996); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CAMERON (Watkin et al., 1996); software used to prepare material for publication: WinGX (Farrugia, 1999).
(C10H8S4Se4)[Fe2(C2N2S3)4] | Z = 1 |
Mr = 1849.06 | F(000) = 884 |
Triclinic, P1 | Dx = 2.488 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.5466 (12) Å | Cell parameters from 8000 reflections |
b = 12.1018 (16) Å | θ = 2–25.9° |
c = 12.9993 (16) Å | µ = 7.37 mm−1 |
α = 109.293 (14)° | T = 160 K |
β = 99.966 (16)° | Block, black |
γ = 95.14 (1)° | 0.15 × 0.12 × 0.10 mm |
V = 1234.2 (3) Å3 |
Stoe IPDS diffractometer | 4503 independent reflections |
Radiation source: fine-focus sealed tube | 3449 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.061 |
φ scans | θmax = 26.1°, θmin = 2.0° |
Absorption correction: part of the refinement model (ΔF) (Parkin et al., 1995) Cubic fit to sinθ/λ with 24 parameters. Correction applied to the full data set. | h = −10→10 |
Tmin = 0.429, Tmax = 0.478 | k = −14→14 |
13154 measured reflections | l = 0→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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0374P)2] where P = (Fo2 + 2Fc2)/3 |
4503 reflections | (Δ/σ)max = 0.001 |
298 parameters | Δρmax = 0.89 e Å−3 |
0 restraints | Δρmin = −0.82 e Å−3 |
Experimental. The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 70 mm. 135 exposures (5 min per exposure) were obtained with 0 < φ < 270° and with the crystals rotated through 2° in φ. Crystal decay was monitored by measuring 200 reflections per image. |
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. |
x | y | z | Uiso*/Ueq | ||
Se1 | 0.10529 (5) | 0.38166 (4) | 0.21999 (4) | 0.01394 (12) | |
Se2 | 0.34615 (5) | 0.37223 (3) | 0.42946 (4) | 0.01019 (11) | |
Se3 | 0.00052 (5) | 0.63386 (4) | 0.38264 (4) | 0.01563 (12) | |
Se4 | 0.24385 (5) | 0.62543 (3) | 0.59168 (4) | 0.01130 (11) | |
S1 | 0.16674 (15) | 0.14254 (11) | 0.06888 (11) | 0.0257 (3) | |
S2 | 0.43263 (13) | 0.13689 (9) | 0.30128 (10) | 0.0164 (3) | |
S4 | 0.16678 (14) | 0.85778 (10) | 0.74588 (11) | 0.0193 (3) | |
S3 | −0.10301 (14) | 0.86119 (9) | 0.51426 (11) | 0.0204 (3) | |
C1 | 0.1935 (5) | 0.4515 (3) | 0.3735 (4) | 0.0102 (9) | |
C2 | 0.1507 (5) | 0.5537 (3) | 0.4395 (4) | 0.0115 (9) | |
C3 | 0.2142 (5) | 0.2510 (3) | 0.2024 (4) | 0.0126 (10) | |
C4 | 0.3173 (5) | 0.2458 (3) | 0.2917 (4) | 0.0109 (9) | |
C5 | 0.0238 (5) | 0.7563 (3) | 0.5211 (4) | 0.0137 (10) | |
C6 | 0.1257 (5) | 0.7522 (3) | 0.6105 (4) | 0.0122 (10) | |
C7 | 0.3525 (6) | 0.0824 (4) | 0.0700 (4) | 0.0207 (11) | |
H7A | 0.3460 | 0.0204 | −0.0035 | 0.025* | |
H7B | 0.4419 | 0.1461 | 0.0814 | 0.025* | |
C8 | 0.3886 (6) | 0.0297 (4) | 0.1601 (4) | 0.0190 (11) | |
H8A | 0.4818 | −0.0125 | 0.1490 | 0.023* | |
H8B | 0.2951 | −0.0296 | 0.1515 | 0.023* | |
C9 | −0.0451 (6) | 0.9745 (4) | 0.6518 (5) | 0.0251 (12) | |
H9A | −0.0638 | 1.0517 | 0.6453 | 0.030* | |
H9B | −0.1158 | 0.9568 | 0.6990 | 0.030* | |
C10 | 0.1282 (6) | 0.9863 (4) | 0.7102 (5) | 0.0236 (12) | |
H10A | 0.1537 | 1.0575 | 0.7791 | 0.028* | |
H10B | 0.1997 | 0.9976 | 0.6609 | 0.028* | |
Fe11 | 0.58858 (7) | 0.53843 (5) | 0.12290 (5) | 0.00994 (15) | |
S11 | 0.67885 (14) | 0.36917 (9) | 0.12074 (10) | 0.0163 (3) | |
S12 | 0.92605 (14) | 0.25783 (10) | −0.12913 (11) | 0.0213 (3) | |
S13 | 0.69297 (12) | 0.54212 (9) | −0.02362 (10) | 0.0112 (2) | |
S14 | 0.60282 (14) | 0.73501 (9) | 0.16334 (10) | 0.0155 (3) | |
S15 | 0.53959 (13) | 0.55249 (9) | 0.28927 (10) | 0.0139 (2) | |
S16 | 0.39416 (16) | 0.87059 (10) | 0.42992 (11) | 0.0227 (3) | |
N11 | 0.8512 (4) | 0.2466 (3) | −0.0236 (3) | 0.0185 (9) | |
N12 | 0.8626 (4) | 0.3795 (3) | −0.1349 (4) | 0.0192 (9) | |
N13 | 0.4192 (4) | 0.7342 (3) | 0.4201 (3) | 0.0170 (9) | |
N14 | 0.4709 (5) | 0.8780 (3) | 0.3240 (3) | 0.0197 (9) | |
C11 | 0.7752 (5) | 0.3375 (4) | 0.0097 (4) | 0.0156 (10) | |
C12 | 0.7827 (5) | 0.4137 (4) | −0.0544 (4) | 0.0128 (10) | |
C13 | 0.4846 (5) | 0.6922 (3) | 0.3339 (4) | 0.0113 (9) | |
C14 | 0.5145 (5) | 0.7748 (4) | 0.2784 (4) | 0.0123 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Se1 | 0.0144 (2) | 0.0144 (2) | 0.0123 (3) | 0.00383 (16) | 0.00031 (18) | 0.00459 (17) |
Se2 | 0.0102 (2) | 0.0106 (2) | 0.0098 (2) | 0.00003 (15) | 0.00195 (17) | 0.00415 (16) |
Se3 | 0.0142 (2) | 0.0163 (2) | 0.0155 (3) | 0.00454 (17) | 0.00081 (19) | 0.00504 (18) |
Se4 | 0.0099 (2) | 0.0115 (2) | 0.0126 (3) | 0.00051 (15) | 0.00286 (17) | 0.00456 (17) |
S1 | 0.0254 (6) | 0.0258 (6) | 0.0149 (7) | 0.0111 (5) | −0.0057 (5) | −0.0039 (5) |
S2 | 0.0185 (6) | 0.0148 (5) | 0.0148 (6) | 0.0065 (4) | 0.0020 (5) | 0.0034 (4) |
S4 | 0.0209 (6) | 0.0168 (5) | 0.0174 (7) | 0.0025 (4) | 0.0064 (5) | 0.0016 (5) |
S3 | 0.0193 (6) | 0.0152 (5) | 0.0295 (8) | 0.0076 (4) | 0.0071 (5) | 0.0092 (5) |
C1 | 0.0038 (18) | 0.014 (2) | 0.014 (2) | −0.0009 (15) | 0.0001 (17) | 0.0085 (17) |
C2 | 0.009 (2) | 0.0103 (19) | 0.015 (3) | −0.0021 (15) | 0.0023 (18) | 0.0044 (17) |
C3 | 0.013 (2) | 0.011 (2) | 0.014 (3) | −0.0008 (16) | 0.0050 (18) | 0.0049 (17) |
C4 | 0.010 (2) | 0.0086 (19) | 0.013 (2) | −0.0018 (15) | 0.0048 (18) | 0.0027 (17) |
C5 | 0.009 (2) | 0.0088 (19) | 0.025 (3) | −0.0024 (15) | 0.0066 (19) | 0.0067 (18) |
C6 | 0.011 (2) | 0.0099 (19) | 0.015 (3) | −0.0018 (16) | 0.0048 (18) | 0.0031 (17) |
C7 | 0.022 (2) | 0.024 (2) | 0.017 (3) | 0.0116 (19) | 0.008 (2) | 0.004 (2) |
C8 | 0.027 (3) | 0.010 (2) | 0.017 (3) | 0.0018 (18) | 0.005 (2) | 0.0007 (18) |
C9 | 0.028 (3) | 0.019 (2) | 0.028 (3) | 0.0059 (19) | 0.013 (2) | 0.004 (2) |
C10 | 0.024 (2) | 0.013 (2) | 0.031 (3) | −0.0016 (18) | 0.010 (2) | 0.003 (2) |
Fe11 | 0.0098 (3) | 0.0112 (3) | 0.0099 (3) | −0.0004 (2) | 0.0027 (2) | 0.0053 (2) |
S11 | 0.0209 (6) | 0.0176 (5) | 0.0154 (6) | 0.0065 (4) | 0.0071 (5) | 0.0099 (4) |
S12 | 0.0189 (6) | 0.0214 (6) | 0.0239 (7) | 0.0064 (4) | 0.0098 (5) | 0.0048 (5) |
S13 | 0.0101 (5) | 0.0126 (5) | 0.0123 (6) | −0.0007 (4) | 0.0047 (4) | 0.0055 (4) |
S14 | 0.0226 (6) | 0.0111 (5) | 0.0142 (6) | −0.0026 (4) | 0.0088 (5) | 0.0052 (4) |
S15 | 0.0214 (6) | 0.0137 (5) | 0.0107 (6) | 0.0039 (4) | 0.0061 (5) | 0.0082 (4) |
S16 | 0.0338 (7) | 0.0173 (6) | 0.0221 (7) | 0.0083 (5) | 0.0156 (6) | 0.0078 (5) |
N11 | 0.0159 (19) | 0.0179 (19) | 0.021 (2) | 0.0064 (15) | 0.0055 (17) | 0.0048 (16) |
N12 | 0.0163 (19) | 0.0186 (19) | 0.020 (2) | 0.0014 (15) | 0.0081 (17) | 0.0024 (16) |
N13 | 0.019 (2) | 0.0163 (18) | 0.019 (2) | 0.0008 (15) | 0.0099 (18) | 0.0088 (16) |
N14 | 0.029 (2) | 0.0166 (19) | 0.016 (2) | 0.0042 (16) | 0.0069 (18) | 0.0076 (16) |
C11 | 0.010 (2) | 0.016 (2) | 0.017 (3) | 0.0002 (17) | 0.0012 (19) | 0.0019 (18) |
C12 | 0.0075 (19) | 0.013 (2) | 0.015 (3) | −0.0027 (16) | −0.0017 (18) | 0.0038 (17) |
C13 | 0.009 (2) | 0.012 (2) | 0.011 (2) | −0.0030 (16) | 0.0004 (18) | 0.0052 (17) |
C14 | 0.014 (2) | 0.011 (2) | 0.014 (3) | −0.0030 (16) | 0.0033 (19) | 0.0085 (17) |
Se1—C3 | 1.875 (4) | C9—H9A | 0.9900 |
Se1—C1 | 1.875 (4) | C9—H9B | 0.9900 |
Se2—C1 | 1.873 (4) | C10—H10A | 0.9900 |
Se2—C4 | 1.892 (4) | C10—H10B | 0.9900 |
Se3—C2 | 1.872 (4) | Fe11—S15 | 2.2282 (15) |
Se3—C5 | 1.880 (5) | Fe11—S11 | 2.2460 (12) |
Se4—C2 | 1.870 (5) | Fe11—S14 | 2.2473 (12) |
Se4—C6 | 1.883 (4) | Fe11—S13 | 2.2500 (14) |
S1—C3 | 1.748 (4) | Fe11—S13i | 2.4656 (12) |
S1—C7 | 1.804 (5) | S11—C11 | 1.735 (5) |
S2—C4 | 1.739 (4) | S12—N12 | 1.634 (4) |
S2—C8 | 1.815 (5) | S12—N11 | 1.650 (5) |
S4—C6 | 1.753 (4) | S13—C12 | 1.753 (4) |
S4—C10 | 1.806 (5) | S13—Fe11i | 2.4656 (12) |
S3—C5 | 1.755 (4) | S14—C14 | 1.737 (5) |
S3—C9 | 1.810 (5) | S15—C13 | 1.734 (4) |
C1—C2 | 1.374 (6) | S16—N14 | 1.648 (5) |
C3—C4 | 1.353 (6) | S16—N13 | 1.650 (4) |
C5—C6 | 1.345 (7) | N11—C11 | 1.316 (5) |
C7—C8 | 1.509 (7) | N12—C12 | 1.321 (6) |
C7—H7A | 0.9900 | N13—C13 | 1.311 (6) |
C7—H7B | 0.9900 | N14—C14 | 1.311 (6) |
C8—H8A | 0.9900 | C11—C12 | 1.437 (7) |
C8—H8B | 0.9900 | C13—C14 | 1.442 (6) |
C9—C10 | 1.513 (7) | ||
Se1···S11ii | 3.622 (1) | Se4···S15iii | 3.519 (1) |
Se3···S15ii | 3.850 (1) | S2···S16iii | 3.585 (2) |
Se2···S15iii | 3.399 (1) | Se1···S13i | 3.624 (2) |
Se4···S11iii | 3.660 (2) | ||
C3—Se1—C1 | 93.91 (18) | S3—C9—H9B | 108.6 |
C1—Se2—C4 | 93.82 (18) | H9A—C9—H9B | 107.6 |
C2—Se3—C5 | 93.52 (19) | C9—C10—S4 | 112.0 (3) |
C2—Se4—C6 | 93.60 (18) | C9—C10—H10A | 109.2 |
C3—S1—C7 | 99.4 (2) | S4—C10—H10A | 109.2 |
C4—S2—C8 | 103.8 (2) | C9—C10—H10B | 109.2 |
C6—S4—C10 | 98.5 (2) | S4—C10—H10B | 109.2 |
C5—S3—C9 | 103.8 (2) | H10A—C10—H10B | 107.9 |
C2—C1—Se2 | 122.7 (3) | S15—Fe11—S11 | 85.95 (5) |
C2—C1—Se1 | 122.5 (3) | S15—Fe11—S14 | 91.82 (5) |
Se2—C1—Se1 | 114.8 (2) | S11—Fe11—S14 | 156.47 (5) |
C1—C2—Se4 | 122.3 (3) | S15—Fe11—S13 | 167.46 (5) |
C1—C2—Se3 | 122.5 (3) | S11—Fe11—S13 | 92.48 (5) |
Se4—C2—Se3 | 115.2 (2) | S14—Fe11—S13 | 84.66 (5) |
C4—C3—S1 | 125.5 (3) | S15—Fe11—S13i | 93.89 (5) |
C4—C3—Se1 | 119.1 (3) | S11—Fe11—S13i | 99.56 (4) |
S1—C3—Se1 | 115.4 (2) | S14—Fe11—S13i | 103.96 (5) |
C3—C4—S2 | 129.5 (3) | S13—Fe11—S13i | 98.64 (4) |
C3—C4—Se2 | 118.2 (3) | C11—S11—Fe11 | 102.66 (16) |
S2—C4—Se2 | 112.3 (2) | N12—S12—N11 | 99.2 (2) |
C6—C5—S3 | 128.6 (4) | C12—S13—Fe11 | 102.29 (17) |
C6—C5—Se3 | 119.0 (3) | C12—S13—Fe11i | 101.60 (13) |
S3—C5—Se3 | 112.4 (3) | Fe11—S13—Fe11i | 81.36 (4) |
C5—C6—S4 | 126.2 (3) | C14—S14—Fe11 | 101.42 (14) |
C5—C6—Se4 | 118.6 (3) | C13—S15—Fe11 | 101.75 (17) |
S4—C6—Se4 | 115.1 (2) | N14—S16—N13 | 98.9 (2) |
C8—C7—S1 | 112.5 (4) | C11—N11—S12 | 107.1 (3) |
C8—C7—H7A | 109.1 | C12—N12—S12 | 106.2 (3) |
S1—C7—H7A | 109.1 | C13—N13—S16 | 106.5 (3) |
C8—C7—H7B | 109.1 | C14—N14—S16 | 106.8 (3) |
S1—C7—H7B | 109.1 | N11—C11—C12 | 112.8 (4) |
H7A—C7—H7B | 107.8 | N11—C11—S11 | 125.6 (4) |
C7—C8—S2 | 114.5 (3) | C12—C11—S11 | 121.6 (3) |
C7—C8—H8A | 108.6 | N12—C12—C11 | 114.8 (4) |
S2—C8—H8A | 108.6 | N12—C12—S13 | 124.2 (4) |
C7—C8—H8B | 108.6 | C11—C12—S13 | 121.0 (4) |
S2—C8—H8B | 108.6 | N13—C13—C14 | 114.2 (4) |
H8A—C8—H8B | 107.6 | N13—C13—S15 | 124.9 (4) |
C10—C9—S3 | 114.8 (3) | C14—C13—S15 | 120.8 (4) |
C10—C9—H9A | 108.6 | N14—C14—C13 | 113.6 (4) |
S3—C9—H9A | 108.6 | N14—C14—S14 | 125.8 (4) |
C10—C9—H9B | 108.6 | C13—C14—S14 | 120.6 (3) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+1. |