The molecule of the title compound, [Cu
2I
2(C
7H
18S
3Si)
2], is dimeric. It lies on an inversion center and contains roughly tetrahedral copper centers surrounded by two thioether groups and two bridging iodo ligands. The Cu
Cu separation, 2.862 (2) Å, is indicative of a weak interaction between the two metal atoms and is not unusual for this type of compound.
Supporting information
CCDC reference: 221614
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (Si-C) = 0.008 Å
- R factor = 0.042
- wR factor = 0.090
- Data-to-parameter ratio = 20.6
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.
Di-µ-iodo-bis{[methyltris(methylthiomethyl)silane-
κ2S,
S']copper(I)}
top
Crystal data top
[Cu2I2(C7H18S3Si)2] | F(000) = 816 |
Mr = 833.85 | Dx = 1.813 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 540 reflections |
a = 9.3372 (1) Å | θ = 2–25° |
b = 12.8346 (3) Å | µ = 3.90 mm−1 |
c = 13.0991 (3) Å | T = 173 K |
β = 103.316 (1)° | Block, colorless |
V = 1527.58 (5) Å3 | 0.20 × 0.10 × 0.08 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2641 independent reflections |
Radiation source: fine-focus sealed tube | 2191 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
φ and ω scans | θmax = 25.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −10→11 |
Tmin = 0.509, Tmax = 0.745 | k = −15→14 |
5836 measured reflections | l = −15→14 |
Refinement top
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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.090 | H-atom parameters constrained |
S = 1.28 | w = 1/[σ2(Fo2) + (0.0168P)2 + 4.7233P] where P = (Fo2 + 2Fc2)/3 |
2641 reflections | (Δ/σ)max = 0.006 |
128 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
I1 | 0.70143 (5) | 0.42962 (4) | 0.59848 (3) | 0.04578 (15) | |
Cu1 | 0.45075 (9) | 0.51598 (7) | 0.59455 (7) | 0.0500 (2) | |
S1 | 0.48949 (19) | 0.66936 (15) | 0.69104 (14) | 0.0502 (4) | |
S2 | 0.2840 (2) | 0.42532 (15) | 0.66557 (14) | 0.0530 (4) | |
S3 | 0.1436 (11) | 0.547 (4) | 0.9347 (13) | 0.101 (7) | 0.75 (10) |
S3A | 0.161 (5) | 0.501 (4) | 0.925 (2) | 0.067 (9) | 0.25 (10) |
Si1 | 0.1804 (2) | 0.63739 (18) | 0.73139 (15) | 0.0509 (5) | |
C1 | 0.3058 (7) | 0.7208 (5) | 0.6733 (5) | 0.0496 (17) | |
H1A | 0.2627 | 0.7289 | 0.5972 | 0.059* | |
H1B | 0.3114 | 0.7909 | 0.7056 | 0.059* | |
C2 | 0.5673 (8) | 0.7572 (6) | 0.6115 (6) | 0.062 (2) | |
H2A | 0.5871 | 0.8245 | 0.6473 | 0.094* | |
H2B | 0.4978 | 0.7669 | 0.5437 | 0.094* | |
H2C | 0.6595 | 0.7280 | 0.6003 | 0.094* | |
C3 | 0.1329 (7) | 0.5156 (6) | 0.6507 (6) | 0.0543 (19) | |
H3A | 0.0494 | 0.4804 | 0.6713 | 0.065* | |
H3B | 0.1004 | 0.5352 | 0.5758 | 0.065* | |
C4 | 0.2050 (10) | 0.3259 (7) | 0.5734 (7) | 0.076 (3) | |
H4A | 0.1332 | 0.2858 | 0.6012 | 0.114* | |
H4B | 0.2829 | 0.2794 | 0.5617 | 0.114* | |
H4C | 0.1557 | 0.3584 | 0.5068 | 0.114* | |
C5 | 0.2716 (8) | 0.6007 (7) | 0.8689 (5) | 0.058 (2) | |
H5A | 0.3504 | 0.5493 | 0.8681 | 0.070* | |
H5B | 0.3175 | 0.6632 | 0.9072 | 0.070* | |
C6 | 0.2613 (12) | 0.4897 (8) | 1.0499 (8) | 0.092 (3) | |
H6A | 0.2011 | 0.4525 | 1.0902 | 0.139* | |
H6B | 0.3172 | 0.5448 | 1.0934 | 0.139* | |
H6C | 0.3297 | 0.4408 | 1.0286 | 0.139* | |
C7 | 0.0083 (8) | 0.7115 (7) | 0.7247 (7) | 0.074 (3) | |
H7A | 0.0306 | 0.7756 | 0.7660 | 0.112* | |
H7B | −0.0606 | 0.6689 | 0.7529 | 0.112* | |
H7C | −0.0361 | 0.7294 | 0.6515 | 0.112* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0369 (2) | 0.0561 (3) | 0.0443 (2) | 0.0061 (2) | 0.00924 (17) | 0.0066 (2) |
Cu1 | 0.0418 (5) | 0.0545 (5) | 0.0551 (5) | 0.0034 (4) | 0.0144 (4) | −0.0014 (4) |
S1 | 0.0426 (9) | 0.0619 (12) | 0.0460 (10) | −0.0022 (8) | 0.0100 (8) | −0.0092 (9) |
S2 | 0.0582 (11) | 0.0580 (11) | 0.0462 (10) | 0.0003 (9) | 0.0190 (8) | 0.0041 (9) |
S3 | 0.074 (3) | 0.16 (2) | 0.079 (4) | −0.011 (6) | 0.038 (3) | 0.027 (7) |
S3A | 0.068 (11) | 0.077 (19) | 0.058 (8) | −0.015 (8) | 0.018 (7) | −0.001 (8) |
Si1 | 0.0398 (10) | 0.0707 (14) | 0.0449 (11) | 0.0001 (9) | 0.0152 (8) | −0.0138 (10) |
C1 | 0.052 (4) | 0.052 (4) | 0.047 (4) | 0.006 (3) | 0.015 (3) | −0.012 (3) |
C2 | 0.056 (5) | 0.071 (5) | 0.062 (5) | −0.018 (4) | 0.017 (4) | −0.012 (4) |
C3 | 0.037 (4) | 0.077 (5) | 0.051 (4) | −0.008 (3) | 0.015 (3) | −0.014 (4) |
C4 | 0.097 (7) | 0.061 (5) | 0.079 (6) | −0.012 (5) | 0.040 (5) | −0.011 (4) |
C5 | 0.051 (4) | 0.079 (6) | 0.047 (4) | −0.006 (4) | 0.015 (3) | −0.011 (4) |
C6 | 0.109 (8) | 0.094 (7) | 0.084 (7) | −0.011 (6) | 0.041 (6) | 0.004 (6) |
C7 | 0.050 (4) | 0.101 (7) | 0.074 (6) | 0.012 (5) | 0.016 (4) | −0.023 (5) |
Geometric parameters (Å, º) top
I1—Cu1 | 2.5796 (9) | C1—H1A | 0.990 |
I1—Cu1i | 2.6916 (10) | C1—H1B | 0.990 |
Cu1—S2 | 2.304 (2) | C2—H2A | 0.980 |
Cu1—S1 | 2.322 (2) | C2—H2B | 0.980 |
Cu1—I1i | 2.6916 (10) | C2—H2C | 0.980 |
Cu1—Cu1i | 2.8633 (17) | C3—H3A | 0.990 |
S1—C2 | 1.798 (8) | C3—H3B | 0.990 |
S1—C1 | 1.803 (7) | C4—H4A | 0.980 |
S2—C4 | 1.794 (8) | C4—H4B | 0.980 |
S2—C3 | 1.801 (7) | C4—H4C | 0.980 |
S3—C5 | 1.767 (13) | C5—H5A | 0.990 |
S3—C6 | 1.81 (2) | C5—H5B | 0.990 |
S3A—C6 | 1.69 (3) | C6—H6A | 0.980 |
S3A—C5 | 1.89 (3) | C6—H6B | 0.980 |
Si1—C7 | 1.853 (8) | C6—H6C | 0.980 |
Si1—C5 | 1.867 (8) | C7—H7A | 0.980 |
Si1—C1 | 1.872 (7) | C7—H7B | 0.980 |
Si1—C3 | 1.882 (7) | C7—H7C | 0.980 |
| | | |
Cu1—I1—Cu1i | 65.76 (3) | S2—C3—H3A | 108.9 |
S2—Cu1—S1 | 104.08 (7) | Si1—C3—H3A | 108.9 |
S2—Cu1—I1 | 117.98 (6) | S2—C3—H3B | 108.9 |
S1—Cu1—I1 | 109.06 (5) | Si1—C3—H3B | 108.9 |
S2—Cu1—I1i | 104.52 (6) | H3A—C3—H3B | 107.7 |
S1—Cu1—I1i | 105.89 (6) | S2—C4—H4A | 109.5 |
I1—Cu1—I1i | 114.24 (3) | S2—C4—H4B | 109.5 |
S2—Cu1—Cu1i | 131.17 (7) | H4A—C4—H4B | 109.5 |
S1—Cu1—Cu1i | 123.47 (7) | S2—C4—H4C | 109.5 |
I1—Cu1—Cu1i | 59.00 (3) | H4A—C4—H4C | 109.5 |
I1i—Cu1—Cu1i | 55.24 (3) | H4B—C4—H4C | 109.5 |
C2—S1—C1 | 101.3 (4) | S3—C5—Si1 | 111.1 (5) |
C2—S1—Cu1 | 104.4 (3) | S3—C5—S3A | 19.5 (6) |
C1—S1—Cu1 | 102.5 (2) | Si1—C5—S3A | 112.2 (10) |
C4—S2—C3 | 101.2 (4) | S3—C5—H5A | 109.4 |
C4—S2—Cu1 | 107.4 (3) | Si1—C5—H5A | 109.4 |
C3—S2—Cu1 | 102.5 (3) | S3A—C5—H5A | 91.4 |
C5—S3—C6 | 102.5 (7) | S3—C5—H5B | 109.4 |
C6—S3A—C5 | 101.8 (13) | Si1—C5—H5B | 109.4 |
C7—Si1—C5 | 111.9 (4) | S3A—C5—H5B | 124.2 |
C7—Si1—C1 | 107.7 (4) | H5A—C5—H5B | 108.0 |
C5—Si1—C1 | 110.4 (3) | S3A—C6—S3 | 20.6 (7) |
C7—Si1—C3 | 108.1 (4) | S3A—C6—H6A | 107.8 |
C5—Si1—C3 | 109.2 (4) | S3—C6—H6A | 109.5 |
C1—Si1—C3 | 109.6 (3) | S3A—C6—H6B | 127.0 |
S1—C1—Si1 | 113.8 (4) | S3—C6—H6B | 109.5 |
S1—C1—H1A | 108.8 | H6A—C6—H6B | 109.5 |
Si1—C1—H1A | 108.8 | S3A—C6—H6C | 91.7 |
S1—C1—H1B | 108.8 | S3—C6—H6C | 109.5 |
Si1—C1—H1B | 108.8 | H6A—C6—H6C | 109.5 |
H1A—C1—H1B | 107.7 | H6B—C6—H6C | 109.5 |
S1—C2—H2A | 109.5 | Si1—C7—H7A | 109.5 |
S1—C2—H2B | 109.5 | Si1—C7—H7B | 109.5 |
H2A—C2—H2B | 109.5 | H7A—C7—H7B | 109.5 |
S1—C2—H2C | 109.5 | Si1—C7—H7C | 109.5 |
H2A—C2—H2C | 109.5 | H7A—C7—H7C | 109.5 |
H2B—C2—H2C | 109.5 | H7B—C7—H7C | 109.5 |
S2—C3—Si1 | 113.3 (4) | | |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1B···I1ii | 0.99 | 3.15 | 4.027 (6) | 149 |
C2—H2A···S2ii | 0.98 | 2.79 | 3.639 (8) | 146 |
Symmetry code: (ii) −x+1, y+1/2, −z+3/2. |