Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807053457/ng2352sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807053457/ng2352Isup2.hkl |
CCDC reference: 672776
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.004 Å
- R factor = 0.017
- wR factor = 0.037
- Data-to-parameter ratio = 19.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT431_ALERT_2_B Short Inter HL..A Contact Br3 .. Br7 .. 3.27 Ang.
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Re - C9 .. 5.50 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Re - C10 .. 7.83 su PLAT431_ALERT_2_C Short Inter HL..A Contact Br1 .. Br5 .. 3.50 Ang.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 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 4 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 0 ALERT type 5 Informative message, check
For general background, see: Merlau et al. (2001); Abou-Hamdan et al. (1998); Keefe et al. (2003); Mines et al. (2002); Sun & Lees (2002). For related structures of diketonato complexes, see: Brasey et al. (2004); Crous et al. (2005); Roodt et al. (2003).
The title complex was synthesized from the literature procedure [Brasey et al., 2004].
H atoms were positioned geometrically and refined using a riding model, with C—H = 0.95Å and with Uiso(H) = 1.2 times Ueq(C aromatic).
Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus (Bruker, 2004) and XPREP (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Fig. 1. : Representation of the title compound (I), showing the numbering scheme and displacement ellipsoids (50% probability). Hydrogen atoms omitted for clarity. |
(C8H20N)[ReBr(C7H2Br3O2)(CO)3] | Z = 2 |
Mr = 838.21 | F(000) = 784 |
Triclinic, P1 | Dx = 2.337 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.9520 (3) Å | Cell parameters from 7112 reflections |
b = 10.0667 (3) Å | θ = 2.5–28.3° |
c = 15.3855 (7) Å | µ = 11.84 mm−1 |
α = 108.391 (2)° | T = 100 K |
β = 92.198 (2)° | Cuboid, red |
γ = 112.888 (1)° | 0.29 × 0.11 × 0.06 mm |
V = 1191.34 (8) Å3 |
Bruker APEXII area-detector diffractometer | 5202 independent reflections |
Radiation source: fine-focus sealed tube | 4815 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
Detector resolution: 512 pixels mm-1 | θmax = 27.0°, θmin = 2.3° |
ϕ and ω scans | h = −11→11 |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | k = −12→12 |
Tmin = 0.242, Tmax = 0.481 | l = −19→19 |
39168 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)] = 0.017 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.037 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0118P)2 + 1.3206P] where P = (Fo2 + 2Fc2)/3 |
5202 reflections | (Δ/σ)max = 0.001 |
262 parameters | Δρmax = 1.07 e Å−3 |
0 restraints | Δρmin = −0.94 e Å−3 |
(C8H20N)[ReBr(C7H2Br3O2)(CO)3] | γ = 112.888 (1)° |
Mr = 838.21 | V = 1191.34 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.9520 (3) Å | Mo Kα radiation |
b = 10.0667 (3) Å | µ = 11.84 mm−1 |
c = 15.3855 (7) Å | T = 100 K |
α = 108.391 (2)° | 0.29 × 0.11 × 0.06 mm |
β = 92.198 (2)° |
Bruker APEXII area-detector diffractometer | 5202 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | 4815 reflections with I > 2σ(I) |
Tmin = 0.242, Tmax = 0.481 | Rint = 0.037 |
39168 measured reflections |
R[F2 > 2σ(F2)] = 0.017 | 0 restraints |
wR(F2) = 0.037 | H-atom parameters constrained |
S = 1.05 | Δρmax = 1.07 e Å−3 |
5202 reflections | Δρmin = −0.94 e Å−3 |
262 parameters |
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 | ||
Re | 0.532795 (13) | 0.457269 (11) | 0.769936 (7) | 0.01223 (4) | |
Br1 | 0.83966 (3) | 0.63718 (3) | 0.855160 (18) | 0.01689 (6) | |
Br7 | 0.72937 (5) | 0.08570 (3) | 0.56481 (2) | 0.03019 (8) | |
O1 | 0.6335 (2) | 0.3195 (2) | 0.67748 (12) | 0.0150 (4) | |
O2 | 0.6044 (2) | 0.5569 (2) | 0.66630 (12) | 0.0136 (4) | |
C1 | 0.6785 (3) | 0.3535 (3) | 0.60665 (17) | 0.0124 (5) | |
C2 | 0.6665 (3) | 0.4926 (3) | 0.60184 (17) | 0.0124 (5) | |
O9 | 0.4074 (2) | 0.6863 (2) | 0.88511 (14) | 0.0226 (4) | |
O8 | 0.1777 (2) | 0.2494 (2) | 0.66949 (14) | 0.0259 (5) | |
O10 | 0.4645 (3) | 0.3058 (2) | 0.91674 (14) | 0.0283 (5) | |
C3 | 0.7218 (3) | 0.5592 (3) | 0.53385 (18) | 0.0136 (5) | |
C7 | 0.7331 (3) | 0.2587 (3) | 0.53904 (18) | 0.0148 (5) | |
C9 | 0.4556 (3) | 0.5991 (3) | 0.84268 (18) | 0.0162 (6) | |
C4 | 0.7840 (3) | 0.5125 (3) | 0.45567 (17) | 0.0144 (5) | |
H4 | 0.8115 | 0.5777 | 0.4217 | 0.017* | |
C10 | 0.4905 (3) | 0.3636 (3) | 0.86116 (19) | 0.0175 (6) | |
C8 | 0.3129 (3) | 0.3267 (3) | 0.70577 (18) | 0.0164 (6) | |
C6 | 0.7882 (3) | 0.2677 (3) | 0.45755 (18) | 0.0155 (5) | |
H6 | 0.8130 | 0.1871 | 0.4233 | 0.019* | |
C5 | 0.8111 (3) | 0.3809 (3) | 0.42055 (17) | 0.0142 (5) | |
Br5 | 0.90032 (3) | 0.35922 (3) | 0.308775 (18) | 0.01785 (6) | |
Br3 | 0.70316 (4) | 0.74797 (3) | 0.554539 (18) | 0.02090 (7) | |
N1 | 0.1588 (3) | 0.8844 (2) | 0.13098 (15) | 0.0137 (4) | |
C13 | 0.2088 (3) | 0.8280 (3) | 0.03798 (18) | 0.0151 (5) | |
H13A | 0.2937 | 0.7940 | 0.0474 | 0.018* | |
H13B | 0.1142 | 0.7387 | −0.0039 | 0.018* | |
C11 | 0.3016 (3) | 1.0234 (3) | 0.19990 (19) | 0.0202 (6) | |
H11A | 0.3313 | 1.1077 | 0.1768 | 0.024* | |
H11B | 0.2648 | 1.0547 | 0.2583 | 0.024* | |
C12 | 0.4542 (4) | 0.9999 (4) | 0.2193 (2) | 0.0267 (7) | |
H12A | 0.5376 | 1.0939 | 0.2636 | 0.040* | |
H12B | 0.4944 | 0.9720 | 0.1624 | 0.040* | |
H12C | 0.4278 | 0.9189 | 0.2442 | 0.040* | |
C17 | 0.0210 (3) | 0.9313 (3) | 0.11604 (18) | 0.0161 (6) | |
H17A | −0.0681 | 0.8443 | 0.0689 | 0.019* | |
H17B | 0.0618 | 1.0145 | 0.0919 | 0.019* | |
C16 | −0.0599 (3) | 0.6199 (3) | 0.1175 (2) | 0.0205 (6) | |
H16A | −0.0858 | 0.5435 | 0.1461 | 0.031* | |
H16B | −0.0524 | 0.5752 | 0.0537 | 0.031* | |
H16C | −0.1451 | 0.6558 | 0.1201 | 0.031* | |
C15 | 0.1032 (3) | 0.7543 (3) | 0.16911 (19) | 0.0185 (6) | |
H15A | 0.1875 | 0.7159 | 0.1674 | 0.022* | |
H15B | 0.0949 | 0.7961 | 0.2339 | 0.022* | |
C18 | −0.0482 (4) | 0.9838 (3) | 0.20244 (19) | 0.0215 (6) | |
H18A | −0.1343 | 1.0112 | 0.1868 | 0.032* | |
H18B | 0.0381 | 1.0720 | 0.2491 | 0.032* | |
H18C | −0.0920 | 0.9015 | 0.2261 | 0.032* | |
C14 | 0.2724 (4) | 0.9454 (3) | −0.00897 (19) | 0.0208 (6) | |
H14A | 0.3007 | 0.8996 | −0.0670 | 0.031* | |
H14B | 0.3684 | 1.0331 | 0.0308 | 0.031* | |
H14C | 0.1884 | 0.9778 | −0.0206 | 0.031* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re | 0.01471 (6) | 0.01303 (6) | 0.00992 (6) | 0.00557 (4) | 0.00251 (4) | 0.00571 (4) |
Br1 | 0.01523 (13) | 0.01916 (13) | 0.01356 (13) | 0.00593 (11) | 0.00087 (10) | 0.00433 (11) |
Br7 | 0.0631 (2) | 0.02116 (15) | 0.01990 (15) | 0.02841 (16) | 0.01035 (15) | 0.01089 (12) |
O1 | 0.0228 (10) | 0.0132 (9) | 0.0120 (9) | 0.0087 (8) | 0.0028 (8) | 0.0069 (8) |
O2 | 0.0185 (10) | 0.0135 (9) | 0.0128 (9) | 0.0088 (8) | 0.0046 (8) | 0.0067 (7) |
C1 | 0.0129 (13) | 0.0099 (12) | 0.0122 (13) | 0.0029 (10) | −0.0015 (10) | 0.0041 (10) |
C2 | 0.0116 (13) | 0.0105 (12) | 0.0118 (13) | 0.0027 (10) | −0.0028 (10) | 0.0028 (10) |
O9 | 0.0237 (11) | 0.0221 (10) | 0.0227 (11) | 0.0113 (9) | 0.0061 (9) | 0.0066 (9) |
O8 | 0.0210 (12) | 0.0282 (11) | 0.0203 (11) | −0.0006 (10) | −0.0023 (9) | 0.0131 (9) |
O10 | 0.0381 (13) | 0.0338 (12) | 0.0223 (11) | 0.0163 (11) | 0.0096 (10) | 0.0201 (10) |
C3 | 0.0175 (14) | 0.0092 (12) | 0.0138 (13) | 0.0065 (11) | −0.0003 (11) | 0.0031 (10) |
C7 | 0.0188 (14) | 0.0102 (12) | 0.0162 (14) | 0.0065 (11) | −0.0002 (11) | 0.0056 (11) |
C9 | 0.0159 (14) | 0.0201 (14) | 0.0135 (13) | 0.0062 (12) | 0.0022 (11) | 0.0092 (11) |
C4 | 0.0167 (14) | 0.0145 (13) | 0.0102 (13) | 0.0037 (11) | 0.0006 (10) | 0.0058 (11) |
C10 | 0.0175 (14) | 0.0182 (14) | 0.0163 (14) | 0.0086 (12) | 0.0021 (11) | 0.0045 (12) |
C8 | 0.0212 (15) | 0.0183 (14) | 0.0119 (13) | 0.0058 (12) | 0.0044 (11) | 0.0111 (11) |
C6 | 0.0174 (14) | 0.0145 (13) | 0.0132 (13) | 0.0085 (11) | 0.0001 (11) | 0.0015 (11) |
C5 | 0.0137 (13) | 0.0186 (13) | 0.0080 (12) | 0.0055 (11) | 0.0015 (10) | 0.0036 (10) |
Br5 | 0.02020 (14) | 0.02090 (14) | 0.01201 (13) | 0.00902 (12) | 0.00518 (11) | 0.00470 (11) |
Br3 | 0.04105 (18) | 0.01303 (13) | 0.01313 (13) | 0.01459 (13) | 0.00591 (12) | 0.00633 (11) |
N1 | 0.0157 (11) | 0.0131 (11) | 0.0106 (11) | 0.0054 (9) | −0.0005 (9) | 0.0034 (9) |
C13 | 0.0171 (14) | 0.0169 (13) | 0.0113 (13) | 0.0084 (11) | 0.0024 (11) | 0.0037 (11) |
C11 | 0.0202 (15) | 0.0169 (14) | 0.0129 (14) | 0.0014 (12) | −0.0006 (11) | 0.0007 (11) |
C12 | 0.0192 (16) | 0.0290 (16) | 0.0213 (16) | 0.0021 (13) | −0.0026 (12) | 0.0068 (13) |
C17 | 0.0212 (14) | 0.0151 (13) | 0.0151 (14) | 0.0104 (12) | 0.0045 (11) | 0.0060 (11) |
C16 | 0.0194 (15) | 0.0137 (13) | 0.0277 (16) | 0.0056 (12) | 0.0065 (12) | 0.0080 (12) |
C15 | 0.0222 (15) | 0.0177 (14) | 0.0176 (14) | 0.0080 (12) | 0.0028 (12) | 0.0096 (12) |
C18 | 0.0271 (16) | 0.0228 (15) | 0.0205 (15) | 0.0138 (13) | 0.0102 (12) | 0.0104 (12) |
C14 | 0.0238 (16) | 0.0256 (15) | 0.0181 (15) | 0.0133 (13) | 0.0091 (12) | 0.0099 (12) |
Re—C9 | 1.894 (3) | N1—C15 | 1.519 (3) |
Re—C8 | 1.897 (3) | C13—C14 | 1.513 (4) |
Re—C10 | 1.898 (3) | C13—H13A | 0.9700 |
Re—O2 | 2.1322 (17) | C13—H13B | 0.9700 |
Re—O1 | 2.1411 (18) | C11—C12 | 1.508 (4) |
Re—Br1 | 2.6270 (3) | C11—H11A | 0.9700 |
Br7—C7 | 1.893 (2) | C11—H11B | 0.9700 |
O1—C1 | 1.276 (3) | C12—H12A | 0.9600 |
O2—C2 | 1.276 (3) | C12—H12B | 0.9600 |
C1—C7 | 1.416 (4) | C12—H12C | 0.9600 |
C1—C2 | 1.470 (3) | C17—C18 | 1.518 (4) |
C2—C3 | 1.419 (4) | C17—H17A | 0.9700 |
O9—C9 | 1.156 (3) | C17—H17B | 0.9700 |
O8—C8 | 1.150 (3) | C16—C15 | 1.513 (4) |
O10—C10 | 1.161 (3) | C16—H16A | 0.9600 |
C3—C4 | 1.370 (4) | C16—H16B | 0.9600 |
C3—Br3 | 1.900 (2) | C16—H16C | 0.9600 |
C7—C6 | 1.381 (4) | C15—H15A | 0.9700 |
C4—C5 | 1.383 (4) | C15—H15B | 0.9700 |
C4—H4 | 0.9300 | C18—H18A | 0.9600 |
C6—C5 | 1.379 (4) | C18—H18B | 0.9600 |
C6—H6 | 0.9300 | C18—H18C | 0.9600 |
C5—Br5 | 1.909 (3) | C14—H14A | 0.9600 |
N1—C11 | 1.511 (3) | C14—H14B | 0.9600 |
N1—C17 | 1.515 (3) | C14—H14C | 0.9600 |
N1—C13 | 1.518 (3) | ||
C9—Re—C8 | 88.62 (12) | C14—C13—H13A | 108.4 |
C9—Re—C10 | 86.86 (11) | N1—C13—H13A | 108.4 |
C8—Re—C10 | 88.99 (11) | C14—C13—H13B | 108.4 |
C9—Re—O2 | 98.38 (9) | N1—C13—H13B | 108.4 |
C8—Re—O2 | 95.05 (9) | H13A—C13—H13B | 107.5 |
C10—Re—O2 | 173.44 (9) | C12—C11—N1 | 115.6 (2) |
C9—Re—O1 | 171.81 (9) | C12—C11—H11A | 108.4 |
C8—Re—O1 | 93.43 (10) | N1—C11—H11A | 108.4 |
C10—Re—O1 | 101.08 (9) | C12—C11—H11B | 108.4 |
O2—Re—O1 | 73.56 (6) | N1—C11—H11B | 108.4 |
C9—Re—Br1 | 92.28 (8) | H11A—C11—H11B | 107.4 |
C8—Re—Br1 | 178.69 (8) | C11—C12—H12A | 109.5 |
C10—Re—Br1 | 92.00 (8) | C11—C12—H12B | 109.5 |
O2—Re—Br1 | 83.89 (5) | H12A—C12—H12B | 109.5 |
O1—Re—Br1 | 85.55 (5) | C11—C12—H12C | 109.5 |
C1—O1—Re | 117.78 (15) | H12A—C12—H12C | 109.5 |
C2—O2—Re | 118.07 (15) | H12B—C12—H12C | 109.5 |
O1—C1—C7 | 120.2 (2) | N1—C17—C18 | 115.0 (2) |
O1—C1—C2 | 115.1 (2) | N1—C17—H17A | 108.5 |
C7—C1—C2 | 124.7 (2) | C18—C17—H17A | 108.5 |
O2—C2—C3 | 119.7 (2) | N1—C17—H17B | 108.5 |
O2—C2—C1 | 115.3 (2) | C18—C17—H17B | 108.5 |
C3—C2—C1 | 125.0 (2) | H17A—C17—H17B | 107.5 |
C4—C3—C2 | 132.3 (2) | C15—C16—H16A | 109.5 |
C4—C3—Br3 | 113.97 (19) | C15—C16—H16B | 109.5 |
C2—C3—Br3 | 113.70 (18) | H16A—C16—H16B | 109.5 |
C6—C7—C1 | 132.4 (2) | C15—C16—H16C | 109.5 |
C6—C7—Br7 | 113.58 (19) | H16A—C16—H16C | 109.5 |
C1—C7—Br7 | 114.01 (19) | H16B—C16—H16C | 109.5 |
O9—C9—Re | 178.3 (2) | C16—C15—N1 | 114.9 (2) |
C3—C4—C5 | 128.5 (2) | C16—C15—H15A | 108.5 |
C3—C4—H4 | 115.8 | N1—C15—H15A | 108.5 |
C5—C4—H4 | 115.8 | C16—C15—H15B | 108.5 |
O10—C10—Re | 179.8 (2) | N1—C15—H15B | 108.5 |
O8—C8—Re | 177.7 (2) | H15A—C15—H15B | 107.5 |
C5—C6—C7 | 128.3 (2) | C17—C18—H18A | 109.5 |
C5—C6—H6 | 115.9 | C17—C18—H18B | 109.5 |
C7—C6—H6 | 115.9 | H18A—C18—H18B | 109.5 |
C6—C5—C4 | 128.5 (2) | C17—C18—H18C | 109.5 |
C6—C5—Br5 | 116.31 (19) | H18A—C18—H18C | 109.5 |
C4—C5—Br5 | 115.13 (19) | H18B—C18—H18C | 109.5 |
C11—N1—C17 | 108.3 (2) | C13—C14—H14A | 109.5 |
C11—N1—C13 | 111.1 (2) | C13—C14—H14B | 109.5 |
C17—N1—C13 | 108.73 (19) | H14A—C14—H14B | 109.5 |
C11—N1—C15 | 109.1 (2) | C13—C14—H14C | 109.5 |
C17—N1—C15 | 111.3 (2) | H14A—C14—H14C | 109.5 |
C13—N1—C15 | 108.26 (19) | H14B—C14—H14C | 109.5 |
C14—C13—N1 | 115.4 (2) | ||
C8—Re—O1—C1 | 91.20 (19) | O1—C1—C7—Br7 | 0.4 (3) |
C10—Re—O1—C1 | −179.16 (19) | C2—C1—C7—Br7 | −178.69 (19) |
O2—Re—O1—C1 | −3.06 (17) | C2—C3—C4—C5 | −0.2 (5) |
Br1—Re—O1—C1 | −87.99 (17) | Br3—C3—C4—C5 | −179.2 (2) |
C9—Re—O2—C2 | 179.53 (18) | C1—C7—C6—C5 | 2.7 (5) |
C8—Re—O2—C2 | −91.12 (19) | Br7—C7—C6—C5 | −177.6 (2) |
O1—Re—O2—C2 | 0.97 (17) | C7—C6—C5—C4 | −0.3 (5) |
Br1—Re—O2—C2 | 88.11 (17) | C7—C6—C5—Br5 | 176.9 (2) |
Re—O1—C1—C7 | −174.73 (18) | C3—C4—C5—C6 | −2.7 (5) |
Re—O1—C1—C2 | 4.5 (3) | C3—C4—C5—Br5 | 180.0 (2) |
Re—O2—C2—C3 | −177.45 (18) | C11—N1—C13—C14 | −58.5 (3) |
Re—O2—C2—C1 | 0.9 (3) | C17—N1—C13—C14 | 60.6 (3) |
O1—C1—C2—O2 | −3.6 (3) | C15—N1—C13—C14 | −178.4 (2) |
C7—C1—C2—O2 | 175.6 (2) | C17—N1—C11—C12 | −176.8 (2) |
O1—C1—C2—C3 | 174.7 (2) | C13—N1—C11—C12 | −57.5 (3) |
C7—C1—C2—C3 | −6.1 (4) | C15—N1—C11—C12 | 61.8 (3) |
O2—C2—C3—C4 | −176.0 (3) | C11—N1—C17—C18 | −61.8 (3) |
C1—C2—C3—C4 | 5.8 (5) | C13—N1—C17—C18 | 177.3 (2) |
O2—C2—C3—Br3 | 3.0 (3) | C15—N1—C17—C18 | 58.2 (3) |
C1—C2—C3—Br3 | −175.16 (19) | C11—N1—C15—C16 | 168.0 (2) |
O1—C1—C7—C6 | −179.8 (3) | C17—N1—C15—C16 | 48.5 (3) |
C2—C1—C7—C6 | 1.1 (5) | C13—N1—C15—C16 | −70.9 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
C18—H18C···O8i | 0.96 | 2.49 | 3.423 (3) | 164 |
C4—H4···O8ii | 0.93 | 2.54 | 3.449 (3) | 167 |
C11—H11B···Br3iii | 0.97 | 2.86 | 3.765 (3) | 155 |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | (C8H20N)[ReBr(C7H2Br3O2)(CO)3] |
Mr | 838.21 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 100 |
a, b, c (Å) | 8.9520 (3), 10.0667 (3), 15.3855 (7) |
α, β, γ (°) | 108.391 (2), 92.198 (2), 112.888 (1) |
V (Å3) | 1191.34 (8) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 11.84 |
Crystal size (mm) | 0.29 × 0.11 × 0.06 |
Data collection | |
Diffractometer | Bruker APEXII area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 1998) |
Tmin, Tmax | 0.242, 0.481 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 39168, 5202, 4815 |
Rint | 0.037 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.017, 0.037, 1.05 |
No. of reflections | 5202 |
No. of parameters | 262 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.07, −0.94 |
Computer programs: APEX2 (Bruker, 2005), SAINT-Plus (Bruker, 2004) and XPREP (Bruker, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg & Putz, 2006).
D—H···A | D—H | H···A | D···A | D—H···A |
C18—H18C···O8i | 0.96 | 2.49 | 3.423 (3) | 163.7 |
C4—H4···O8ii | 0.93 | 2.54 | 3.449 (3) | 167.3 |
C11—H11B···Br3iii | 0.97 | 2.86 | 3.765 (3) | 154.9 |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y+2, −z+1. |
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The title compound, (I), is presented as an example of a fac-ReI(CO)3 fragment containing the highly substituted 3,5,7-tribromotropolonato moiety, see Figure 1. These rhenium systems are commonly employed in catalysis [Merlau et al., 2001; Abou-Hamdan et al., 1998], sensing devices [Keefe et al., 2003; Mines et al., 2002] and building blocks in self-assembled metallomacrocycles [Sun & Lees, 2002]. A closely related derivative of 3-hydroxy-1,2,4-benzotriazine-4-one [Brasey et al., 2004] have been reported.
The title complex crystallizes in the asymmetric unit with two independent ionic fragmets. The effect of the small bite angle of the tribromotropolonato moiety can be observed from the slightly distorted octahedral geometry around the ReI metal centre, see Table 1.
An interesting observation in the title complex is the effect of weak intermolecular hydrogen bonding contacts between the cationic [NEt4]+ and anionic [ReBr(CO)3TropBr3]- moieties, see Table 2. This solid state ordering is further enhanced through Br..Br interactions between pairs of the bromonated tropolonato moieties, Br3..Br7 [x, 1 + y, z] 3.2675 (5)/%A 168.4 (1)/% and Br7..Br3 [x, -1 + y, z] 3.2675 (5)/%A 166.2 (1)/%, respectively. The bromido ligand on the metal centre is also involved in Br..Br interactions with the brominated tropolonato ligand, Br5..Br1 [2 - x, 1 - y, 1 - z] 3.4962 (4)/%A 165.1 (1)/%.