Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803020385/om6176sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803020385/om6176Isup2.hkl |
CCDC reference: 225690
Key indicators
- Single-crystal X-ray study
- T = 175 K
- Mean (C-C) = 0.003 Å
- R factor = 0.026
- wR factor = 0.065
- Data-to-parameter ratio = 20.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.98
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT142_ALERT_4_C su on b - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe2 - S4 = 6.93 su PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 Cl O4
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 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 1 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 3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and DIAMOND (Crystal Impact, 1997); software used to prepare material for publication: SHELXTL.
[Fe(C4H8S2)3](ClO4)2 | Z = 2 |
Mr = 615.42 | F(000) = 632 |
Triclinic, P1 | Dx = 1.856 Mg m−3 |
a = 8.7854 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.3729 (1) Å | Cell parameters from 7696 reflections |
c = 11.5862 (3) Å | θ = 2.4–28.2° |
α = 85.828 (1)° | µ = 1.54 mm−1 |
β = 84.276 (1)° | T = 175 K |
γ = 73.129 (1)° | Rod, purple |
V = 1101.13 (4) Å3 | 0.40 × 0.16 × 0.16 mm |
Bruker SMART 1K Platform CCD diffractometer | 5333 independent reflections |
Radiation source: sealed tube | 4592 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
ω scans | θmax = 28.2°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.602, Tmax = 0.782 | k = −15→15 |
11893 measured reflections | l = −15→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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0306P)2 + 0.7215P] where P = (Fo2 + 2Fc2)/3 |
5333 reflections | (Δ/σ)max = 0.001 |
265 parameters | Δρmax = 0.49 e Å−3 |
0 restraints | Δρmin = −0.39 e Å−3 |
Experimental. The crystal was mounted on the tip of a glass fiber with epoxy resin. The first 50 frames of data were recollected for a decay correction. The decay correction was applied simultaneously with the absorption correction in SADABS. No formal measure of the extent of decay is printed out by this program. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 σ(I). Note that the absorption correction parameters Tmin and Tmax also reflect beam corrections, etc. As a result, the numerical values for Tmin and Tmax may differ from expected values based solely absorption effects and crystal size. |
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 | ||
Fe1 | 0.0000 | 0.5000 | 0.5000 | 0.01361 (8) | |
S1 | 0.10779 (5) | 0.33499 (4) | 0.39173 (4) | 0.01826 (10) | |
S2 | −0.00776 (5) | 0.37392 (4) | 0.65879 (4) | 0.01752 (9) | |
S3 | 0.24629 (5) | 0.50261 (4) | 0.53612 (4) | 0.01883 (10) | |
C1 | 0.1449 (2) | 0.39865 (19) | 0.74216 (16) | 0.0218 (4) | |
H1A | 0.1008 | 0.4769 | 0.7821 | 0.026* | |
H1B | 0.1729 | 0.3314 | 0.8024 | 0.026* | |
C2 | 0.2949 (2) | 0.40335 (19) | 0.66720 (17) | 0.0228 (4) | |
H2B | 0.3556 | 0.3192 | 0.6447 | 0.027* | |
H2A | 0.3633 | 0.4350 | 0.7124 | 0.027* | |
C3 | 0.3736 (2) | 0.4092 (2) | 0.42241 (17) | 0.0247 (4) | |
H3B | 0.3704 | 0.4601 | 0.3491 | 0.030* | |
H3A | 0.4851 | 0.3833 | 0.4441 | 0.030* | |
C4 | 0.3237 (2) | 0.29531 (19) | 0.40196 (17) | 0.0232 (4) | |
H4B | 0.3541 | 0.2337 | 0.4667 | 0.028* | |
H4A | 0.3802 | 0.2584 | 0.3292 | 0.028* | |
C5 | 0.0564 (3) | 0.21273 (18) | 0.48285 (18) | 0.0243 (4) | |
H5A | −0.0578 | 0.2195 | 0.4781 | 0.029* | |
H5B | 0.1200 | 0.1322 | 0.4532 | 0.029* | |
C6 | 0.0867 (2) | 0.21777 (17) | 0.60848 (17) | 0.0230 (4) | |
H6B | 0.2030 | 0.1950 | 0.6161 | 0.028* | |
H6A | 0.0423 | 0.1582 | 0.6570 | 0.028* | |
Fe2 | 0.0000 | 0.0000 | 0.0000 | 0.01309 (8) | |
S4 | 0.08608 (5) | −0.04736 (4) | −0.18516 (4) | 0.01747 (9) | |
S5 | 0.04576 (5) | −0.20238 (4) | 0.04961 (4) | 0.01756 (9) | |
S6 | 0.25281 (5) | −0.01284 (4) | 0.03583 (4) | 0.01659 (9) | |
C7 | 0.1230 (2) | −0.28424 (17) | −0.08465 (17) | 0.0237 (4) | |
H7A | 0.2411 | −0.3111 | −0.0894 | 0.028* | |
H7B | 0.0855 | −0.3585 | −0.0833 | 0.028* | |
C8 | 0.0673 (2) | −0.20204 (18) | −0.19052 (17) | 0.0229 (4) | |
H8A | −0.0459 | −0.1965 | −0.1979 | 0.027* | |
H8B | 0.1303 | −0.2405 | −0.2607 | 0.027* | |
C9 | 0.3035 (2) | −0.07575 (19) | −0.19587 (16) | 0.0217 (4) | |
H9A | 0.3557 | −0.1642 | −0.1796 | 0.026* | |
H9B | 0.3410 | −0.0535 | −0.2756 | 0.026* | |
C10 | 0.3493 (2) | −0.00022 (19) | −0.10977 (17) | 0.0222 (4) | |
H10A | 0.3195 | 0.0872 | −0.1376 | 0.027* | |
H10B | 0.4665 | −0.0279 | −0.1061 | 0.027* | |
C11 | 0.3464 (2) | −0.17570 (17) | 0.07298 (17) | 0.0200 (4) | |
H11A | 0.3999 | −0.2179 | 0.0018 | 0.024* | |
H11B | 0.4287 | −0.1827 | 0.1276 | 0.024* | |
C12 | 0.2244 (2) | −0.23779 (17) | 0.12791 (16) | 0.0201 (4) | |
H12A | 0.1936 | −0.2117 | 0.2087 | 0.024* | |
H12B | 0.2737 | −0.3279 | 0.1311 | 0.024* | |
Cl1 | 0.30207 (6) | 0.38295 (4) | 0.06047 (4) | 0.02500 (11) | |
O1 | 0.3533 (2) | 0.42020 (17) | −0.05372 (14) | 0.0420 (4) | |
O2 | 0.1616 (2) | 0.47322 (17) | 0.10453 (19) | 0.0544 (5) | |
O3 | 0.4290 (2) | 0.3686 (2) | 0.13454 (16) | 0.0523 (5) | |
O4 | 0.2706 (3) | 0.26688 (18) | 0.0576 (2) | 0.0699 (7) | |
Cl2 | 0.34074 (6) | −0.11507 (5) | 0.40054 (4) | 0.02949 (12) | |
O5 | 0.2244 (2) | −0.03581 (17) | 0.32941 (16) | 0.0493 (5) | |
O6 | 0.4977 (2) | −0.11091 (17) | 0.35675 (19) | 0.0475 (5) | |
O7 | 0.3077 (3) | −0.0775 (3) | 0.51736 (17) | 0.0751 (8) | |
O8 | 0.3329 (2) | −0.24011 (17) | 0.39528 (18) | 0.0462 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.01319 (16) | 0.01318 (16) | 0.01443 (16) | −0.00380 (13) | −0.00159 (12) | 0.00028 (13) |
S1 | 0.0199 (2) | 0.0169 (2) | 0.0172 (2) | −0.00342 (17) | −0.00225 (16) | −0.00204 (17) |
S2 | 0.0178 (2) | 0.0172 (2) | 0.0170 (2) | −0.00497 (17) | −0.00073 (16) | 0.00171 (16) |
S3 | 0.0160 (2) | 0.0215 (2) | 0.0201 (2) | −0.00706 (17) | −0.00296 (16) | 0.00073 (17) |
C1 | 0.0213 (9) | 0.0261 (10) | 0.0170 (8) | −0.0047 (8) | −0.0042 (7) | 0.0005 (7) |
C2 | 0.0188 (9) | 0.0278 (10) | 0.0202 (9) | −0.0032 (8) | −0.0068 (7) | 0.0021 (8) |
C3 | 0.0155 (9) | 0.0343 (11) | 0.0221 (9) | −0.0052 (8) | 0.0015 (7) | 0.0007 (8) |
C4 | 0.0164 (9) | 0.0276 (10) | 0.0208 (9) | 0.0005 (8) | 0.0018 (7) | −0.0019 (8) |
C5 | 0.0301 (10) | 0.0160 (9) | 0.0283 (10) | −0.0087 (8) | −0.0017 (8) | −0.0022 (8) |
C6 | 0.0266 (10) | 0.0147 (8) | 0.0253 (10) | −0.0040 (7) | 0.0003 (8) | 0.0026 (7) |
Fe2 | 0.01195 (16) | 0.01345 (16) | 0.01425 (17) | −0.00399 (13) | −0.00220 (12) | −0.00002 (13) |
S4 | 0.0166 (2) | 0.0201 (2) | 0.0155 (2) | −0.00447 (17) | −0.00337 (16) | 0.00013 (17) |
S5 | 0.0180 (2) | 0.0152 (2) | 0.0202 (2) | −0.00575 (16) | −0.00237 (16) | 0.00045 (17) |
S6 | 0.0139 (2) | 0.0186 (2) | 0.0183 (2) | −0.00575 (16) | −0.00336 (16) | −0.00028 (17) |
C7 | 0.0284 (10) | 0.0168 (9) | 0.0261 (10) | −0.0053 (8) | −0.0033 (8) | −0.0057 (8) |
C8 | 0.0251 (10) | 0.0232 (9) | 0.0229 (9) | −0.0087 (8) | −0.0035 (7) | −0.0079 (8) |
C9 | 0.0153 (8) | 0.0302 (10) | 0.0179 (9) | −0.0050 (7) | 0.0009 (7) | 0.0007 (8) |
C10 | 0.0174 (9) | 0.0276 (10) | 0.0222 (9) | −0.0088 (8) | −0.0004 (7) | 0.0037 (8) |
C11 | 0.0163 (8) | 0.0194 (9) | 0.0219 (9) | −0.0011 (7) | −0.0041 (7) | 0.0018 (7) |
C12 | 0.0218 (9) | 0.0189 (9) | 0.0190 (9) | −0.0046 (7) | −0.0055 (7) | 0.0043 (7) |
Cl1 | 0.0231 (2) | 0.0201 (2) | 0.0295 (2) | −0.00415 (18) | 0.00428 (18) | −0.00343 (19) |
O1 | 0.0421 (10) | 0.0510 (11) | 0.0236 (8) | −0.0009 (8) | 0.0001 (7) | 0.0034 (7) |
O2 | 0.0432 (11) | 0.0352 (10) | 0.0678 (13) | 0.0074 (8) | 0.0245 (10) | −0.0081 (9) |
O3 | 0.0500 (11) | 0.0745 (14) | 0.0290 (9) | −0.0097 (10) | −0.0118 (8) | −0.0011 (9) |
O4 | 0.0516 (13) | 0.0328 (10) | 0.128 (2) | −0.0236 (9) | 0.0269 (13) | −0.0229 (12) |
Cl2 | 0.0218 (2) | 0.0371 (3) | 0.0235 (2) | 0.0040 (2) | −0.00704 (18) | −0.0057 (2) |
O5 | 0.0474 (11) | 0.0436 (10) | 0.0435 (10) | 0.0193 (8) | −0.0279 (9) | −0.0148 (8) |
O6 | 0.0299 (9) | 0.0364 (9) | 0.0743 (14) | −0.0093 (7) | −0.0015 (9) | 0.0059 (9) |
O7 | 0.0717 (15) | 0.106 (2) | 0.0287 (10) | 0.0142 (14) | −0.0152 (10) | −0.0267 (11) |
O8 | 0.0331 (9) | 0.0423 (10) | 0.0636 (12) | −0.0131 (8) | −0.0052 (8) | 0.0068 (9) |
Fe1—S1 | 2.2508 (4) | Fe2—S6ii | 2.2613 (4) |
Fe1—S1i | 2.2508 (4) | Fe2—S6 | 2.2613 (4) |
Fe1—S3i | 2.2534 (4) | S4—C8 | 1.820 (2) |
Fe1—S3 | 2.2534 (4) | S4—C9 | 1.8358 (19) |
Fe1—S2i | 2.2568 (4) | S5—C12 | 1.8199 (19) |
Fe1—S2 | 2.2568 (4) | S5—C7 | 1.839 (2) |
S1—C5 | 1.819 (2) | S6—C10 | 1.8262 (19) |
S1—C4 | 1.8318 (19) | S6—C11 | 1.8338 (19) |
S2—C1 | 1.8241 (19) | C7—C8 | 1.518 (3) |
S2—C6 | 1.8387 (19) | C7—H7A | 0.9900 |
S3—C3 | 1.826 (2) | C7—H7B | 0.9900 |
S3—C2 | 1.834 (2) | C8—H8A | 0.9900 |
C1—C2 | 1.517 (3) | C8—H8B | 0.9900 |
C1—H1A | 0.9900 | C9—C10 | 1.517 (3) |
C1—H1B | 0.9900 | C9—H9A | 0.9900 |
C2—H2B | 0.9900 | C9—H9B | 0.9900 |
C2—H2A | 0.9900 | C10—H10A | 0.9900 |
C3—C4 | 1.524 (3) | C10—H10B | 0.9900 |
C3—H3B | 0.9900 | C11—C12 | 1.514 (3) |
C3—H3A | 0.9900 | C11—H11A | 0.9900 |
C4—H4B | 0.9900 | C11—H11B | 0.9900 |
C4—H4A | 0.9900 | C12—H12A | 0.9900 |
C5—C6 | 1.514 (3) | C12—H12B | 0.9900 |
C5—H5A | 0.9900 | Cl1—O4 | 1.4285 (19) |
C5—H5B | 0.9900 | Cl1—O1 | 1.4293 (17) |
C6—H6B | 0.9900 | Cl1—O2 | 1.4329 (16) |
C6—H6A | 0.9900 | Cl1—O3 | 1.4396 (19) |
Fe2—S4 | 2.2523 (4) | Cl2—O7 | 1.4257 (19) |
Fe2—S4ii | 2.2523 (4) | Cl2—O6 | 1.4341 (18) |
Fe2—S5ii | 2.2597 (4) | Cl2—O5 | 1.4359 (17) |
Fe2—S5 | 2.2597 (4) | Cl2—O8 | 1.4495 (19) |
S1—Fe1—S1i | 180.000 (19) | S4—Fe2—S6ii | 90.575 (16) |
S1—Fe1—S3i | 90.079 (17) | S4ii—Fe2—S6ii | 89.425 (16) |
S1i—Fe1—S3i | 89.921 (17) | S5ii—Fe2—S6ii | 89.604 (16) |
S1—Fe1—S3 | 89.921 (17) | S5—Fe2—S6ii | 90.396 (16) |
S1i—Fe1—S3 | 90.079 (17) | S4—Fe2—S6 | 89.425 (16) |
S3i—Fe1—S3 | 180.0 | S4ii—Fe2—S6 | 90.575 (16) |
S1—Fe1—S2i | 90.266 (16) | S5ii—Fe2—S6 | 90.396 (16) |
S1i—Fe1—S2i | 89.734 (16) | S5—Fe2—S6 | 89.604 (16) |
S3i—Fe1—S2i | 89.625 (16) | S6ii—Fe2—S6 | 180.00 (2) |
S3—Fe1—S2i | 90.375 (16) | C8—S4—C9 | 101.95 (9) |
S1—Fe1—S2 | 89.734 (16) | C8—S4—Fe2 | 102.73 (7) |
S1i—Fe1—S2 | 90.266 (16) | C9—S4—Fe2 | 106.19 (6) |
S3i—Fe1—S2 | 90.375 (16) | C12—S5—C7 | 101.59 (9) |
S3—Fe1—S2 | 89.625 (16) | C12—S5—Fe2 | 103.24 (6) |
S2i—Fe1—S2 | 180.0 | C7—S5—Fe2 | 106.18 (7) |
C5—S1—C4 | 101.48 (10) | C10—S6—C11 | 100.08 (9) |
C5—S1—Fe1 | 102.13 (7) | C10—S6—Fe2 | 102.62 (6) |
C4—S1—Fe1 | 106.00 (7) | C11—S6—Fe2 | 105.62 (6) |
C1—S2—C6 | 102.19 (9) | C8—C7—S5 | 110.81 (13) |
C1—S2—Fe1 | 102.56 (7) | C8—C7—H7A | 109.5 |
C6—S2—Fe1 | 105.18 (7) | S5—C7—H7A | 109.5 |
C3—S3—C2 | 102.38 (9) | C8—C7—H7B | 109.5 |
C3—S3—Fe1 | 102.73 (7) | S5—C7—H7B | 109.5 |
C2—S3—Fe1 | 105.95 (6) | H7A—C7—H7B | 108.1 |
C2—C1—S2 | 112.73 (13) | C7—C8—S4 | 113.61 (13) |
C2—C1—H1A | 109.0 | C7—C8—H8A | 108.8 |
S2—C1—H1A | 109.0 | S4—C8—H8A | 108.8 |
C2—C1—H1B | 109.0 | C7—C8—H8B | 108.8 |
S2—C1—H1B | 109.0 | S4—C8—H8B | 108.8 |
H1A—C1—H1B | 107.8 | H8A—C8—H8B | 107.7 |
C1—C2—S3 | 111.10 (13) | C10—C9—S4 | 110.16 (13) |
C1—C2—H2B | 109.4 | C10—C9—H9A | 109.6 |
S3—C2—H2B | 109.4 | S4—C9—H9A | 109.6 |
C1—C2—H2A | 109.4 | C10—C9—H9B | 109.6 |
S3—C2—H2A | 109.4 | S4—C9—H9B | 109.6 |
H2B—C2—H2A | 108.0 | H9A—C9—H9B | 108.1 |
C4—C3—S3 | 112.97 (13) | C9—C10—S6 | 112.71 (13) |
C4—C3—H3B | 109.0 | C9—C10—H10A | 109.1 |
S3—C3—H3B | 109.0 | S6—C10—H10A | 109.1 |
C4—C3—H3A | 109.0 | C9—C10—H10B | 109.1 |
S3—C3—H3A | 109.0 | S6—C10—H10B | 109.1 |
H3B—C3—H3A | 107.8 | H10A—C10—H10B | 107.8 |
C3—C4—S1 | 110.65 (13) | C12—C11—S6 | 111.25 (13) |
C3—C4—H4B | 109.5 | C12—C11—H11A | 109.4 |
S1—C4—H4B | 109.5 | S6—C11—H11A | 109.4 |
C3—C4—H4A | 109.5 | C12—C11—H11B | 109.4 |
S1—C4—H4A | 109.5 | S6—C11—H11B | 109.4 |
H4B—C4—H4A | 108.1 | H11A—C11—H11B | 108.0 |
C6—C5—S1 | 112.22 (13) | C11—C12—S5 | 113.08 (13) |
C6—C5—H5A | 109.2 | C11—C12—H12A | 109.0 |
S1—C5—H5A | 109.2 | S5—C12—H12A | 109.0 |
C6—C5—H5B | 109.2 | C11—C12—H12B | 109.0 |
S1—C5—H5B | 109.2 | S5—C12—H12B | 109.0 |
H5A—C5—H5B | 107.9 | H12A—C12—H12B | 107.8 |
C5—C6—S2 | 109.70 (13) | O4—Cl1—O1 | 109.62 (14) |
C5—C6—H6B | 109.7 | O4—Cl1—O2 | 110.05 (12) |
S2—C6—H6B | 109.7 | O1—Cl1—O2 | 110.32 (12) |
C5—C6—H6A | 109.7 | O4—Cl1—O3 | 108.30 (15) |
S2—C6—H6A | 109.7 | O1—Cl1—O3 | 108.49 (11) |
H6B—C6—H6A | 108.2 | O2—Cl1—O3 | 110.02 (13) |
S4—Fe2—S4ii | 180.000 (8) | O7—Cl2—O6 | 110.30 (14) |
S4—Fe2—S5ii | 90.412 (16) | O7—Cl2—O5 | 109.62 (12) |
S4ii—Fe2—S5ii | 89.588 (16) | O6—Cl2—O5 | 109.88 (12) |
S4—Fe2—S5 | 89.588 (16) | O7—Cl2—O8 | 110.06 (15) |
S4ii—Fe2—S5 | 90.412 (16) | O6—Cl2—O8 | 108.34 (11) |
S5ii—Fe2—S5 | 180.000 (7) | O5—Cl2—O8 | 108.61 (11) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x, −y, −z. |
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