Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005149/ob6606sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005149/ob6606Isup2.hkl |
CCDC reference: 601223
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (S-C) = 0.003 Å
- R factor = 0.023
- wR factor = 0.056
- Data-to-parameter ratio = 28.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb1 - S1 .. 6.56 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb2 - S3 .. 9.17 su
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART-W2K/NT (Bruker, 2003); cell refinement: SAINT-W2K/NT (Bruker, 2003); data reduction: SAINT-W2K/NT; program(s) used to solve structure: SHELXTL-NT (Bruker, 2003); program(s) used to refine structure: SHELXTL-NT; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL-NT.
[Nb2Cl6(C2H6S)3] | F(000) = 1144 |
Mr = 584.90 | Dx = 2.020 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 7953 reflections |
a = 8.0002 (8) Å | θ = 2.6–27.9° |
b = 11.3868 (11) Å | µ = 2.33 mm−1 |
c = 21.446 (2) Å | T = 173 K |
β = 100.040 (2)° | Block, violet |
V = 1923.7 (3) Å3 | 0.41 × 0.40 × 0.39 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 4586 independent reflections |
Radiation source: fine-focus sealed tube | 4293 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
Detector resolution: 8.366 pixels mm-1 | θmax = 27.9°, θmin = 1.9° |
φ and ω scans | h = −7→10 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −13→14 |
Tmin = 0.390, Tmax = 0.403 | l = −28→25 |
13709 measured reflections |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.056 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0255P)2 + 0.7014P] where P = (Fo2 + 2Fc2)/3 |
4586 reflections | (Δ/σ)max < 0.001 |
160 parameters | Δρmax = 0.40 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
Geometry. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 5.6539 (0.0011) x + 3.8229 (0.0018) y + 15.7935 (0.0029) z = 6.3837 (0.0014) * 0.0398 (0.0003) Cl5 * 0.0320 (0.0003) Cl6 * 0.0214 (0.0003) Cl3 * 0.0329 (0.0003) Cl4 * -0.1261 (0.0003) N b2 Rms deviation of fitted atoms = 0.0633 2.0994 (0.0013) x - 8.9584 (0.0015) y + 10.8179 (0.0033) z = 1.2709 (0.0015) Angle to previous plane (with approximate e.s.d.) = 84.17 (0.01) * -0.0487 (0.0003) Cl1 * -0.0324 (0.0003) Cl2 * -0.0213 (0.0003) Cl3 * -0.0420 (0.0003) Cl4 * 0.1445 (0.0003) N b1 Rms deviation of fitted atoms = 0.0728 |
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 | ||
C1 | 0.0180 (3) | 0.4861 (3) | 0.22772 (15) | 0.0466 (7) | |
H1A | −0.0422 | 0.4910 | 0.2637 | 0.070* | |
H1B | −0.0049 | 0.4099 | 0.2068 | 0.070* | |
H1C | −0.0212 | 0.5491 | 0.1976 | 0.070* | |
C2 | 0.2499 (5) | 0.6379 (3) | 0.29723 (16) | 0.0571 (9) | |
H2A | 0.2103 | 0.7014 | 0.2674 | 0.086* | |
H2B | 0.3670 | 0.6536 | 0.3178 | 0.086* | |
H2C | 0.1769 | 0.6335 | 0.3294 | 0.086* | |
C3 | 0.4407 (3) | 0.0023 (2) | 0.35202 (12) | 0.0313 (5) | |
H3A | 0.5156 | −0.0165 | 0.3218 | 0.047* | |
H3B | 0.3221 | −0.0024 | 0.3307 | 0.047* | |
H3C | 0.4601 | −0.0539 | 0.3872 | 0.047* | |
C4 | 0.7109 (3) | 0.1425 (2) | 0.41139 (12) | 0.0322 (5) | |
H4A | 0.7341 | 0.0829 | 0.4448 | 0.048* | |
H4B | 0.7510 | 0.2192 | 0.4286 | 0.048* | |
H4C | 0.7701 | 0.1216 | 0.3766 | 0.048* | |
C5 | 0.0669 (5) | 0.2174 (3) | 0.57307 (14) | 0.0523 (9) | |
H5A | 0.1801 | 0.1933 | 0.5944 | 0.079* | |
H5B | 0.0066 | 0.1494 | 0.5520 | 0.079* | |
H5C | 0.0031 | 0.2491 | 0.6044 | 0.079* | |
C6 | 0.1982 (3) | 0.4386 (2) | 0.56653 (13) | 0.0373 (6) | |
H6A | 0.1270 | 0.4648 | 0.5967 | 0.056* | |
H6B | 0.2242 | 0.5056 | 0.5412 | 0.056* | |
H6C | 0.3040 | 0.4054 | 0.5897 | 0.056* | |
Cl1 | 0.27498 (8) | 0.21144 (6) | 0.23471 (3) | 0.03306 (13) | |
Cl2 | 0.62429 (7) | 0.38770 (5) | 0.31438 (3) | 0.02848 (12) | |
Cl3 | 0.05892 (6) | 0.30142 (5) | 0.35368 (3) | 0.02479 (11) | |
Cl4 | 0.35345 (7) | 0.45582 (5) | 0.42247 (3) | 0.02528 (11) | |
Cl5 | 0.15869 (7) | 0.06066 (5) | 0.44884 (3) | 0.03027 (13) | |
Cl6 | 0.51466 (8) | 0.23977 (5) | 0.53243 (3) | 0.03222 (13) | |
Nb1 | 0.35266 (2) | 0.322651 (17) | 0.329589 (9) | 0.01881 (6) | |
Nb2 | 0.29486 (2) | 0.245439 (16) | 0.442356 (9) | 0.01880 (6) | |
S1 | 0.24129 (8) | 0.50127 (6) | 0.25530 (3) | 0.03072 (13) | |
S2 | 0.48567 (7) | 0.14932 (5) | 0.38231 (3) | 0.02141 (11) | |
S3 | 0.08671 (8) | 0.32853 (6) | 0.51513 (3) | 0.02923 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0321 (14) | 0.0514 (18) | 0.0520 (17) | 0.0103 (12) | −0.0045 (13) | 0.0202 (14) |
C2 | 0.077 (2) | 0.0322 (16) | 0.057 (2) | 0.0041 (15) | −0.0006 (18) | 0.0097 (14) |
C3 | 0.0367 (13) | 0.0250 (12) | 0.0347 (13) | 0.0027 (10) | 0.0125 (11) | 0.0004 (10) |
C4 | 0.0205 (11) | 0.0420 (14) | 0.0323 (13) | 0.0061 (10) | −0.0002 (10) | 0.0068 (11) |
C5 | 0.086 (2) | 0.0441 (17) | 0.0354 (16) | −0.0268 (16) | 0.0334 (16) | −0.0066 (13) |
C6 | 0.0425 (15) | 0.0332 (14) | 0.0377 (14) | −0.0052 (11) | 0.0111 (12) | −0.0112 (11) |
Cl1 | 0.0355 (3) | 0.0403 (3) | 0.0219 (3) | 0.0005 (3) | 0.0010 (2) | −0.0053 (2) |
Cl2 | 0.0218 (3) | 0.0330 (3) | 0.0318 (3) | −0.0034 (2) | 0.0079 (2) | 0.0048 (2) |
Cl3 | 0.0166 (2) | 0.0343 (3) | 0.0231 (3) | 0.0008 (2) | 0.0024 (2) | 0.0028 (2) |
Cl4 | 0.0307 (3) | 0.0212 (3) | 0.0247 (3) | −0.0037 (2) | 0.0068 (2) | −0.0005 (2) |
Cl5 | 0.0345 (3) | 0.0249 (3) | 0.0334 (3) | −0.0080 (2) | 0.0114 (2) | 0.0013 (2) |
Cl6 | 0.0316 (3) | 0.0389 (3) | 0.0229 (3) | 0.0017 (2) | −0.0045 (2) | 0.0017 (2) |
Nb1 | 0.01661 (10) | 0.02206 (10) | 0.01772 (10) | 0.00097 (7) | 0.00287 (7) | 0.00293 (7) |
Nb2 | 0.01862 (10) | 0.02035 (10) | 0.01727 (10) | −0.00148 (7) | 0.00269 (7) | 0.00165 (7) |
S1 | 0.0295 (3) | 0.0354 (3) | 0.0288 (3) | 0.0091 (2) | 0.0092 (2) | 0.0132 (2) |
S2 | 0.0190 (3) | 0.0230 (3) | 0.0220 (3) | 0.00182 (19) | 0.0030 (2) | 0.0032 (2) |
S3 | 0.0260 (3) | 0.0391 (3) | 0.0235 (3) | −0.0026 (2) | 0.0067 (2) | −0.0047 (2) |
C1—S1 | 1.789 (3) | C5—H5C | 0.9800 |
C1—H1A | 0.9800 | C6—S3 | 1.800 (3) |
C1—H1B | 0.9800 | C6—H6A | 0.9800 |
C1—H1C | 0.9800 | C6—H6B | 0.9800 |
C2—S1 | 1.793 (3) | C6—H6C | 0.9800 |
C2—H2A | 0.9800 | Cl1—Nb1 | 2.3853 (6) |
C2—H2B | 0.9800 | Cl2—Nb1 | 2.3715 (6) |
C2—H2C | 0.9800 | Cl3—Nb1 | 2.5043 (6) |
C3—S2 | 1.809 (2) | Cl4—Nb1 | 2.5026 (6) |
C3—H3A | 0.9800 | Cl3—Nb2 | 2.5168 (6) |
C3—H3B | 0.9800 | Cl4—Nb2 | 2.4920 (6) |
C3—H3C | 0.9800 | Cl5—Nb2 | 2.3845 (6) |
C4—S2 | 1.803 (2) | Cl6—Nb2 | 2.3756 (6) |
C4—H4A | 0.9800 | Nb1—S2 | 2.4262 (6) |
C4—H4B | 0.9800 | Nb1—S1 | 2.6409 (6) |
C4—H4C | 0.9800 | Nb1—Nb2 | 2.6880 (3) |
C5—S3 | 1.800 (3) | Nb2—S2 | 2.4233 (6) |
C5—H5A | 0.9800 | Nb2—S3 | 2.6477 (6) |
C5—H5B | 0.9800 | ||
S1—C1—H1A | 109.5 | S2—Nb1—Cl3 | 100.160 (19) |
S1—C1—H1B | 109.5 | Cl4—Nb1—Cl3 | 76.495 (19) |
H1A—C1—H1B | 109.5 | Cl2—Nb1—S1 | 84.11 (2) |
S1—C1—H1C | 109.5 | Cl1—Nb1—S1 | 83.33 (2) |
H1A—C1—H1C | 109.5 | S2—Nb1—S1 | 169.14 (2) |
H1B—C1—H1C | 109.5 | Cl4—Nb1—S1 | 88.13 (2) |
S1—C2—H2A | 109.5 | Cl3—Nb1—S1 | 88.211 (19) |
S1—C2—H2B | 109.5 | Cl2—Nb1—Nb2 | 122.097 (16) |
H2A—C2—H2B | 109.5 | Cl1—Nb1—Nb2 | 122.260 (19) |
S1—C2—H2C | 109.5 | S2—Nb1—Nb2 | 56.285 (14) |
H2A—C2—H2C | 109.5 | Cl4—Nb1—Nb2 | 57.248 (15) |
H2B—C2—H2C | 109.5 | Cl3—Nb1—Nb2 | 57.857 (13) |
S2—C3—H3A | 109.5 | S1—Nb1—Nb2 | 134.573 (16) |
S2—C3—H3B | 109.5 | Cl6—Nb2—Cl5 | 102.10 (2) |
H3A—C3—H3B | 109.5 | Cl6—Nb2—S2 | 88.53 (2) |
S2—C3—H3C | 109.5 | Cl5—Nb2—S2 | 88.22 (2) |
H3A—C3—H3C | 109.5 | Cl6—Nb2—Cl4 | 91.75 (2) |
H3B—C3—H3C | 109.5 | Cl5—Nb2—Cl4 | 163.68 (2) |
S2—C4—H4A | 109.5 | S2—Nb2—Cl4 | 100.870 (19) |
S2—C4—H4B | 109.5 | Cl6—Nb2—Cl3 | 166.57 (2) |
H4A—C4—H4B | 109.5 | Cl5—Nb2—Cl3 | 88.71 (2) |
S2—C4—H4C | 109.5 | S2—Nb2—Cl3 | 99.89 (2) |
H4A—C4—H4C | 109.5 | Cl4—Nb2—Cl3 | 76.461 (19) |
H4B—C4—H4C | 109.5 | Cl6—Nb2—S3 | 89.02 (2) |
S3—C5—H5A | 109.5 | Cl5—Nb2—S3 | 86.58 (2) |
S3—C5—H5B | 109.5 | S2—Nb2—S3 | 173.66 (2) |
H5A—C5—H5B | 109.5 | Cl4—Nb2—S3 | 85.05 (2) |
S3—C5—H5C | 109.5 | Cl3—Nb2—S3 | 83.63 (2) |
H5A—C5—H5C | 109.5 | Cl6—Nb2—Nb1 | 121.427 (18) |
H5B—C5—H5C | 109.5 | Cl5—Nb2—Nb1 | 119.542 (16) |
S3—C6—H6A | 109.5 | S2—Nb2—Nb1 | 56.391 (14) |
S3—C6—H6B | 109.5 | Cl4—Nb2—Nb1 | 57.632 (13) |
H6A—C6—H6B | 109.5 | Cl3—Nb2—Nb1 | 57.408 (14) |
S3—C6—H6C | 109.5 | S3—Nb2—Nb1 | 129.643 (17) |
H6A—C6—H6C | 109.5 | C1—S1—C2 | 101.44 (16) |
H6B—C6—H6C | 109.5 | C1—S1—Nb1 | 109.72 (10) |
Nb1—Cl3—Nb2 | 64.735 (15) | C2—S1—Nb1 | 112.74 (11) |
Nb2—Cl4—Nb1 | 65.120 (15) | C4—S2—C3 | 102.02 (12) |
Cl2—Nb1—Cl1 | 99.05 (2) | C4—S2—Nb2 | 121.33 (9) |
Cl2—Nb1—S2 | 88.87 (2) | C3—S2—Nb2 | 120.31 (8) |
Cl1—Nb1—S2 | 89.63 (2) | C4—S2—Nb1 | 121.81 (9) |
Cl2—Nb1—Cl4 | 92.58 (2) | C3—S2—Nb1 | 122.82 (9) |
Cl1—Nb1—Cl4 | 164.76 (2) | Nb2—S2—Nb1 | 67.324 (16) |
S2—Nb1—Cl4 | 100.48 (2) | C6—S3—C5 | 99.25 (14) |
Cl2—Nb1—Cl3 | 166.87 (2) | C6—S3—Nb2 | 108.33 (9) |
Cl1—Nb1—Cl3 | 90.60 (2) | C5—S3—Nb2 | 107.22 (11) |
Nb2—Cl4—Nb1—Cl2 | −127.117 (18) | Cl2—Nb1—S1—C1 | 165.16 (12) |
Nb2—Cl4—Nb1—Cl1 | 93.06 (8) | Cl1—Nb1—S1—C1 | 65.30 (12) |
Nb2—Cl4—Nb1—S2 | −37.794 (18) | S2—Nb1—S1—C1 | 115.20 (16) |
Nb2—Cl4—Nb1—Cl3 | 60.257 (16) | Cl4—Nb1—S1—C1 | −102.05 (12) |
Nb2—Cl4—Nb1—S1 | 148.867 (18) | Cl3—Nb1—S1—C1 | −25.51 (12) |
Nb2—Cl3—Nb1—Cl2 | −93.95 (9) | Nb2—Nb1—S1—C1 | −64.43 (12) |
Nb2—Cl3—Nb1—Cl1 | 128.60 (2) | Cl2—Nb1—S1—C2 | −82.59 (14) |
Nb2—Cl3—Nb1—S2 | 38.869 (18) | Cl1—Nb1—S1—C2 | 177.55 (14) |
Nb2—Cl3—Nb1—Cl4 | −59.589 (17) | S2—Nb1—S1—C2 | −132.55 (17) |
Nb2—Cl3—Nb1—S1 | −148.092 (19) | Cl4—Nb1—S1—C2 | 10.20 (14) |
Nb1—Cl4—Nb2—Cl6 | 126.74 (2) | Cl3—Nb1—S1—C2 | 86.74 (14) |
Nb1—Cl4—Nb2—Cl5 | −84.99 (7) | Nb2—Nb1—S1—C2 | 47.82 (14) |
Nb1—Cl4—Nb2—S2 | 37.905 (18) | Cl6—Nb2—S2—C4 | −15.56 (10) |
Nb1—Cl4—Nb2—Cl3 | −59.778 (16) | Cl5—Nb2—S2—C4 | −117.71 (10) |
Nb1—Cl4—Nb2—S3 | −144.399 (18) | Cl4—Nb2—S2—C4 | 75.95 (10) |
Nb1—Cl3—Nb2—Cl6 | 89.27 (9) | Cl3—Nb2—S2—C4 | 153.91 (10) |
Nb1—Cl3—Nb2—Cl5 | −126.855 (18) | Nb1—Nb2—S2—C4 | 114.49 (10) |
Nb1—Cl3—Nb2—S2 | −38.887 (18) | Cl6—Nb2—S2—C3 | 114.10 (10) |
Nb1—Cl3—Nb2—Cl4 | 60.024 (16) | Cl5—Nb2—S2—C3 | 11.95 (10) |
Nb1—Cl3—Nb2—S3 | 146.446 (19) | Cl4—Nb2—S2—C3 | −154.40 (10) |
Cl2—Nb1—Nb2—Cl6 | 0.28 (3) | Cl3—Nb2—S2—C3 | −76.43 (10) |
Cl1—Nb1—Nb2—Cl6 | 128.26 (3) | Nb1—Nb2—S2—C3 | −115.86 (10) |
S2—Nb1—Nb2—Cl6 | 63.75 (3) | Cl6—Nb2—S2—Nb1 | −130.043 (19) |
Cl4—Nb1—Nb2—Cl6 | −69.83 (2) | Cl5—Nb2—S2—Nb1 | 127.804 (19) |
Cl3—Nb1—Nb2—Cl6 | −164.20 (3) | Cl4—Nb2—S2—Nb1 | −38.539 (18) |
S1—Nb1—Nb2—Cl6 | −116.33 (3) | Cl3—Nb2—S2—Nb1 | 39.427 (18) |
Cl2—Nb1—Nb2—Cl5 | −128.67 (3) | Cl2—Nb1—S2—C4 | 16.88 (10) |
Cl1—Nb1—Nb2—Cl5 | −0.69 (3) | Cl1—Nb1—S2—C4 | 115.93 (10) |
S2—Nb1—Nb2—Cl5 | −65.20 (3) | Cl4—Nb1—S2—C4 | −75.54 (10) |
Cl4—Nb1—Nb2—Cl5 | 161.23 (3) | Cl3—Nb1—S2—C4 | −153.52 (10) |
Cl3—Nb1—Nb2—Cl5 | 66.85 (2) | S1—Nb1—S2—C4 | 66.49 (16) |
S1—Nb1—Nb2—Cl5 | 114.72 (3) | Nb2—Nb1—S2—C4 | −113.82 (10) |
Cl2—Nb1—Nb2—S2 | −63.47 (3) | Cl2—Nb1—S2—C3 | −116.88 (10) |
Cl1—Nb1—Nb2—S2 | 64.51 (3) | Cl1—Nb1—S2—C3 | −17.83 (10) |
Cl4—Nb1—Nb2—S2 | −133.58 (2) | Cl4—Nb1—S2—C3 | 150.70 (10) |
Cl3—Nb1—Nb2—S2 | 132.05 (2) | Cl3—Nb1—S2—C3 | 72.71 (10) |
S1—Nb1—Nb2—S2 | 179.92 (3) | S1—Nb1—S2—C3 | −67.27 (15) |
Cl2—Nb1—Nb2—Cl4 | 70.11 (2) | Nb2—Nb1—S2—C3 | 112.41 (10) |
Cl1—Nb1—Nb2—Cl4 | −161.92 (3) | Cl2—Nb1—S2—Nb2 | 130.702 (18) |
S2—Nb1—Nb2—Cl4 | 133.58 (2) | Cl1—Nb1—S2—Nb2 | −130.24 (2) |
Cl3—Nb1—Nb2—Cl4 | −94.37 (2) | Cl4—Nb1—S2—Nb2 | 38.287 (18) |
S1—Nb1—Nb2—Cl4 | −46.50 (3) | Cl3—Nb1—S2—Nb2 | −39.701 (18) |
Cl2—Nb1—Nb2—Cl3 | 164.48 (3) | S1—Nb1—S2—Nb2 | −179.69 (11) |
Cl1—Nb1—Nb2—Cl3 | −67.54 (3) | Cl6—Nb2—S3—C6 | 43.26 (10) |
S2—Nb1—Nb2—Cl3 | −132.05 (2) | Cl5—Nb2—S3—C6 | 145.44 (10) |
Cl4—Nb1—Nb2—Cl3 | 94.37 (2) | Cl4—Nb2—S3—C6 | −48.59 (10) |
S1—Nb1—Nb2—Cl3 | 47.87 (3) | Cl3—Nb2—S3—C6 | −125.48 (10) |
Cl2—Nb1—Nb2—S3 | 118.97 (3) | Nb1—Nb2—S3—C6 | −88.27 (10) |
Cl1—Nb1—Nb2—S3 | −113.05 (3) | Cl6—Nb2—S3—C5 | −63.00 (12) |
S2—Nb1—Nb2—S3 | −177.56 (3) | Cl5—Nb2—S3—C5 | 39.18 (12) |
Cl4—Nb1—Nb2—S3 | 48.87 (3) | Cl4—Nb2—S3—C5 | −154.85 (12) |
Cl3—Nb1—Nb2—S3 | −45.51 (3) | Cl3—Nb2—S3—C5 | 128.26 (12) |
S1—Nb1—Nb2—S3 | 2.36 (3) | Nb1—Nb2—S3—C5 | 165.47 (12) |
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