Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016258/bt6311sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016258/bt6311Isup2.hkl |
CCDC reference: 221658
Data collection: R-AXIS Control Software (Molecular Structure Corporation, 1994); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: XS in SHELXTL (Sheldrick, 1997); program(s) used to refine structure: XL in SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: XL in SHELXTL.
[Ti2Cl6O(C2H6S)4] | F(000) = 1160 |
Mr = 573.01 | Dx = 1.620 Mg m−3 |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 221 reflections |
a = 25.311 (5) Å | θ = 1.6–22.7° |
b = 9.801 (2) Å | µ = 1.71 mm−1 |
c = 9.4720 (19) Å | T = 140 K |
V = 2349.7 (8) Å3 | Block, orange |
Z = 4 | 0.40 × 0.35 × 0.30 mm |
Rigaku R-AXIS-IIc diffractometer | 4021 reflections with I > 2σ(I) |
Radiation source: rotating anode | Rint = 0.053 |
Graphite monochromator | θmax = 25.4°, θmin = 3.0° |
image–plate oscillation photos scans | h = −30→30 |
11796 measured reflections | k = −11→11 |
4350 independent reflections | l = −11→11 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.029 | H-atom parameters constrained |
wR(F2) = 0.077 | w = 1/[σ2(Fo2) + (0.0544P)2 + 0.4789P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
4153 reflections | Δρmax = 0.29 e Å−3 |
201 parameters | Δρmin = −0.46 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 1846 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.45 (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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ti1 | 0.593491 (19) | 0.66459 (5) | 0.72521 (6) | 0.02846 (13) | |
Cl1 | 0.59434 (3) | 0.49193 (8) | 0.88274 (9) | 0.03829 (18) | |
Cl2 | 0.66945 (3) | 0.60197 (8) | 0.60999 (11) | 0.04270 (19) | |
Cl3 | 0.50865 (3) | 0.73528 (8) | 0.76186 (9) | 0.03869 (18) | |
S1 | 0.54541 (3) | 0.49035 (9) | 0.55118 (9) | 0.03780 (18) | |
C11 | 0.59109 (16) | 0.3521 (4) | 0.5210 (5) | 0.0519 (10) | |
H11A | 0.6204 | 0.3844 | 0.4661 | 0.078* | |
H11B | 0.5735 | 0.2801 | 0.4710 | 0.078* | |
H11C | 0.6037 | 0.3183 | 0.6100 | 0.078* | |
C12 | 0.49657 (16) | 0.4004 (4) | 0.6533 (5) | 0.0542 (10) | |
H12A | 0.4686 | 0.4619 | 0.6786 | 0.081* | |
H12B | 0.5126 | 0.3648 | 0.7374 | 0.081* | |
H12C | 0.4825 | 0.3266 | 0.5984 | 0.081* | |
S2 | 0.58655 (3) | 0.80773 (8) | 0.48956 (9) | 0.03339 (17) | |
C21 | 0.64171 (13) | 0.9240 (4) | 0.4858 (4) | 0.0408 (8) | |
H21A | 0.6741 | 0.8731 | 0.4849 | 0.061* | |
H21B | 0.6407 | 0.9812 | 0.5681 | 0.061* | |
H21C | 0.6397 | 0.9796 | 0.4026 | 0.061* | |
C22 | 0.53303 (13) | 0.9276 (4) | 0.4906 (4) | 0.0447 (8) | |
H22A | 0.5001 | 0.8793 | 0.4927 | 0.067* | |
H22B | 0.5347 | 0.9830 | 0.4071 | 0.067* | |
H22C | 0.5357 | 0.9849 | 0.5725 | 0.067* | |
O1 | 0.62347 (9) | 0.7974 (2) | 0.8315 (3) | 0.0374 (5) | |
Ti2 | 0.64473 (2) | 0.94158 (5) | 0.93019 (6) | 0.02713 (12) | |
Cl4 | 0.58629 (3) | 0.92278 (8) | 1.11430 (9) | 0.03542 (17) | |
Cl5 | 0.59995 (3) | 1.10740 (7) | 0.81455 (9) | 0.03686 (17) | |
Cl6 | 0.72394 (3) | 0.96757 (7) | 0.81372 (9) | 0.03655 (17) | |
S3 | 0.68496 (3) | 1.14255 (8) | 1.09402 (9) | 0.03569 (17) | |
C31 | 0.71321 (15) | 1.2685 (3) | 0.9783 (5) | 0.0441 (8) | |
H31A | 0.7441 | 1.2316 | 0.9336 | 0.066* | |
H31B | 0.7228 | 1.3478 | 1.0320 | 0.066* | |
H31C | 0.6878 | 1.2935 | 0.9076 | 0.066* | |
C32 | 0.63002 (15) | 1.2401 (4) | 1.1591 (4) | 0.0478 (9) | |
H32A | 0.6101 | 1.1858 | 1.2245 | 0.072* | |
H32B | 0.6078 | 1.2662 | 1.0816 | 0.072* | |
H32C | 0.6428 | 1.3204 | 1.2060 | 0.072* | |
S4 | 0.70410 (3) | 0.79506 (9) | 1.10212 (10) | 0.04073 (19) | |
C41 | 0.66427 (14) | 0.6608 (3) | 1.1719 (4) | 0.0414 (7) | |
H41A | 0.6381 | 0.6984 | 1.2341 | 0.062* | |
H41B | 0.6862 | 0.5982 | 1.2234 | 0.062* | |
H41C | 0.6471 | 0.6135 | 1.0959 | 0.062* | |
C42A | 0.7424 (10) | 0.680 (2) | 0.9811 (16) | 0.052 (4) | 0.59 (7) |
H42A | 0.7676 | 0.7324 | 0.9289 | 0.079* | 0.59 (7) |
H42B | 0.7185 | 0.6357 | 0.9167 | 0.079* | 0.59 (7) |
H42C | 0.7605 | 0.6118 | 1.0359 | 0.079* | 0.59 (7) |
C42B | 0.7576 (13) | 0.722 (4) | 1.023 (6) | 0.079 (10) | 0.41 (7) |
H42D | 0.7797 | 0.7921 | 0.9834 | 0.118* | 0.41 (7) |
H42E | 0.7459 | 0.6624 | 0.9485 | 0.118* | 0.41 (7) |
H42F | 0.7773 | 0.6707 | 1.0910 | 0.118* | 0.41 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0260 (2) | 0.0280 (2) | 0.0314 (3) | 0.00019 (19) | −0.0008 (2) | 0.0002 (2) |
Cl1 | 0.0482 (4) | 0.0308 (4) | 0.0360 (4) | −0.0010 (3) | −0.0080 (3) | 0.0050 (3) |
Cl2 | 0.0296 (4) | 0.0421 (4) | 0.0563 (5) | 0.0054 (3) | 0.0064 (4) | −0.0009 (4) |
Cl3 | 0.0297 (4) | 0.0458 (4) | 0.0405 (4) | 0.0048 (3) | 0.0050 (3) | 0.0062 (3) |
S1 | 0.0429 (4) | 0.0376 (4) | 0.0329 (4) | −0.0071 (3) | −0.0068 (3) | 0.0000 (3) |
C11 | 0.067 (3) | 0.0419 (19) | 0.047 (2) | 0.0001 (17) | −0.0063 (18) | −0.0094 (17) |
C12 | 0.051 (2) | 0.058 (2) | 0.054 (2) | −0.0256 (19) | −0.0043 (18) | −0.0012 (18) |
S2 | 0.0319 (4) | 0.0379 (4) | 0.0303 (4) | −0.0005 (3) | 0.0007 (3) | 0.0027 (3) |
C21 | 0.0378 (18) | 0.0435 (19) | 0.0409 (18) | −0.0047 (14) | 0.0020 (14) | 0.0075 (15) |
C22 | 0.0333 (17) | 0.057 (2) | 0.044 (2) | 0.0085 (15) | 0.0002 (15) | 0.0133 (17) |
O1 | 0.0397 (12) | 0.0319 (10) | 0.0406 (13) | 0.0012 (9) | −0.0018 (10) | 0.0020 (10) |
Ti2 | 0.0268 (2) | 0.0268 (3) | 0.0278 (3) | −0.00061 (19) | −0.00061 (19) | 0.0018 (2) |
Cl4 | 0.0301 (3) | 0.0406 (4) | 0.0356 (4) | 0.0016 (3) | 0.0038 (3) | 0.0071 (3) |
Cl5 | 0.0422 (4) | 0.0327 (4) | 0.0357 (4) | 0.0048 (3) | −0.0053 (3) | 0.0046 (3) |
Cl6 | 0.0347 (4) | 0.0386 (4) | 0.0364 (4) | −0.0038 (3) | 0.0069 (3) | 0.0008 (3) |
S3 | 0.0371 (4) | 0.0341 (4) | 0.0358 (4) | −0.0002 (3) | −0.0052 (3) | −0.0033 (3) |
C31 | 0.0377 (17) | 0.0355 (16) | 0.059 (2) | −0.0066 (14) | 0.0009 (16) | −0.0070 (16) |
C32 | 0.057 (2) | 0.0389 (18) | 0.048 (2) | 0.0041 (16) | 0.0133 (18) | −0.0074 (15) |
S4 | 0.0314 (4) | 0.0430 (4) | 0.0478 (5) | 0.0007 (3) | −0.0070 (4) | 0.0125 (4) |
C41 | 0.0397 (17) | 0.0404 (18) | 0.0443 (19) | 0.0027 (15) | −0.0039 (15) | 0.0082 (15) |
C42A | 0.042 (7) | 0.051 (7) | 0.065 (6) | 0.023 (5) | 0.015 (4) | 0.026 (5) |
C42B | 0.036 (10) | 0.080 (14) | 0.12 (2) | 0.013 (10) | 0.028 (11) | 0.034 (17) |
Ti1—O1 | 1.812 (2) | Ti2—Cl4 | 2.2940 (10) |
Ti1—Cl1 | 2.2562 (10) | Ti2—Cl6 | 2.3025 (10) |
Ti1—Cl3 | 2.2829 (9) | Ti2—S4 | 2.6405 (10) |
Ti1—Cl2 | 2.2943 (10) | Ti2—S3 | 2.7064 (10) |
Ti1—S2 | 2.6422 (10) | S3—C32 | 1.797 (4) |
Ti1—S1 | 2.6672 (10) | S3—C31 | 1.799 (4) |
S1—C12 | 1.800 (4) | C31—H31A | 0.9600 |
S1—C11 | 1.804 (4) | C31—H31B | 0.9600 |
C11—H11A | 0.9600 | C31—H31C | 0.9600 |
C11—H11B | 0.9600 | C32—H32A | 0.9600 |
C11—H11C | 0.9600 | C32—H32B | 0.9600 |
C12—H12A | 0.9600 | C32—H32C | 0.9600 |
C12—H12B | 0.9600 | S4—C42B | 1.71 (3) |
C12—H12C | 0.9600 | S4—C41 | 1.785 (4) |
S2—C22 | 1.793 (3) | S4—C42A | 1.880 (13) |
S2—C21 | 1.803 (3) | C41—H41A | 0.9600 |
C21—H21A | 0.9600 | C41—H41B | 0.9600 |
C21—H21B | 0.9600 | C41—H41C | 0.9600 |
C21—H21C | 0.9600 | C42A—H42A | 0.9600 |
C22—H22A | 0.9600 | C42A—H42B | 0.9600 |
C22—H22B | 0.9600 | C42A—H42C | 0.9600 |
C22—H22C | 0.9600 | C42B—H42D | 0.9600 |
O1—Ti2 | 1.778 (2) | C42B—H42E | 0.9600 |
Ti2—Cl5 | 2.2639 (9) | C42B—H42F | 0.9600 |
O1—Ti1—Cl1 | 99.64 (8) | Cl5—Ti2—Cl6 | 97.16 (4) |
O1—Ti1—Cl3 | 95.24 (8) | Cl4—Ti2—Cl6 | 159.15 (4) |
Cl1—Ti1—Cl3 | 97.82 (4) | O1—Ti2—S4 | 93.69 (8) |
O1—Ti1—Cl2 | 96.06 (8) | Cl5—Ti2—S4 | 166.83 (4) |
Cl1—Ti1—Cl2 | 96.08 (4) | Cl4—Ti2—S4 | 81.62 (3) |
Cl3—Ti1—Cl2 | 160.34 (4) | Cl6—Ti2—S4 | 81.96 (3) |
O1—Ti1—S2 | 96.64 (8) | O1—Ti2—S3 | 173.68 (8) |
Cl1—Ti1—S2 | 163.25 (4) | Cl5—Ti2—S3 | 86.75 (3) |
Cl3—Ti1—S2 | 84.53 (3) | Cl4—Ti2—S3 | 82.25 (3) |
Cl2—Ti1—S2 | 78.22 (3) | Cl6—Ti2—S3 | 82.34 (3) |
O1—Ti1—S1 | 173.87 (8) | S4—Ti2—S3 | 80.10 (3) |
Cl1—Ti1—S1 | 86.15 (3) | C32—S3—C31 | 98.70 (18) |
Cl3—Ti1—S1 | 81.90 (3) | C32—S3—Ti2 | 107.02 (14) |
Cl2—Ti1—S1 | 85.25 (4) | C31—S3—Ti2 | 107.44 (13) |
S2—Ti1—S1 | 77.73 (3) | S3—C31—H31A | 109.5 |
C12—S1—C11 | 99.1 (2) | S3—C31—H31B | 109.5 |
C12—S1—Ti1 | 107.14 (14) | H31A—C31—H31B | 109.5 |
C11—S1—Ti1 | 106.63 (13) | S3—C31—H31C | 109.5 |
S1—C11—H11A | 109.5 | H31A—C31—H31C | 109.5 |
S1—C11—H11B | 109.5 | H31B—C31—H31C | 109.5 |
H11A—C11—H11B | 109.5 | S3—C32—H32A | 109.5 |
S1—C11—H11C | 109.5 | S3—C32—H32B | 109.5 |
H11A—C11—H11C | 109.5 | H32A—C32—H32B | 109.5 |
H11B—C11—H11C | 109.5 | S3—C32—H32C | 109.5 |
S1—C12—H12A | 109.5 | H32A—C32—H32C | 109.5 |
S1—C12—H12B | 109.5 | H32B—C32—H32C | 109.5 |
H12A—C12—H12B | 109.5 | C42B—S4—C41 | 107.6 (12) |
S1—C12—H12C | 109.5 | C41—S4—C42A | 94.2 (8) |
H12A—C12—H12C | 109.5 | C42B—S4—Ti2 | 114.0 (15) |
H12B—C12—H12C | 109.5 | C41—S4—Ti2 | 107.95 (12) |
C22—S2—C21 | 99.83 (18) | C42A—S4—Ti2 | 104.1 (5) |
C22—S2—Ti1 | 113.18 (13) | S4—C41—H41A | 109.5 |
C21—S2—Ti1 | 107.50 (12) | S4—C41—H41B | 109.5 |
S2—C21—H21A | 109.5 | H41A—C41—H41B | 109.5 |
S2—C21—H21B | 109.5 | S4—C41—H41C | 109.5 |
H21A—C21—H21B | 109.5 | H41A—C41—H41C | 109.5 |
S2—C21—H21C | 109.5 | H41B—C41—H41C | 109.5 |
H21A—C21—H21C | 109.5 | S4—C42A—H42A | 109.5 |
H21B—C21—H21C | 109.5 | S4—C42A—H42B | 109.5 |
S2—C22—H22A | 109.5 | H42A—C42A—H42B | 109.5 |
S2—C22—H22B | 109.5 | S4—C42A—H42C | 109.5 |
H22A—C22—H22B | 109.5 | H42A—C42A—H42C | 109.5 |
S2—C22—H22C | 109.5 | H42B—C42A—H42C | 109.5 |
H22A—C22—H22C | 109.5 | S4—C42B—H42D | 109.5 |
H22B—C22—H22C | 109.5 | S4—C42B—H42E | 109.5 |
Ti2—O1—Ti1 | 171.86 (14) | H42D—C42B—H42E | 109.5 |
O1—Ti2—Cl5 | 99.47 (8) | S4—C42B—H42F | 109.5 |
O1—Ti2—Cl4 | 98.09 (8) | H42D—C42B—H42F | 109.5 |
Cl5—Ti2—Cl4 | 95.90 (4) | H42E—C42B—H42F | 109.5 |
O1—Ti2—Cl6 | 95.71 (8) |