Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807060485/hb2661sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807060485/hb2661Isup2.hkl |
CCDC reference: 625468
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.012 Å
- R factor = 0.040
- wR factor = 0.112
- Data-to-parameter ratio = 15.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Sb1 - Br1 .. 15.35 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Sb1 - Br2 .. 14.51 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Sb1 - Br3 .. 15.58 su
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.95 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Sb1 - Br4 .. 8.22 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Sb1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C25 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 12
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 9
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The corresponding SbF3 complex with 1,10-phenanthroline was reported by Bertazzi et al. (1983).
Antimony tribromide (180.7 mg, 0.5 mmol) was dissolved in methanol (20 ml) and 1,10-phenanthroline (99.1 mg, 0.5 mmol) was added with stirring at room temperature. The resulting orange–red solution was allowed to react for five hours and was then filtered. Yellow blocks of (I) were obtained by slow evaporation of an ethanol/dichloromethane (1:2 v/v) solution over a period of two weeks (yield 88%. m.p. 430 K). Anal. Calcd (%) for C25H19Br4Cl2N4Sb: C 33.82; H 2.16; N 6.31. Found: C 33.94; H 2.05; N 6.45.
The H atom bound to N1 was located in a difference map, relocated in an idealized position (N—H = 0.86 Å) and refined as riding with Uiso(H) = 1.2Ueq(N). The C-bound H atoms were placed in calculated positions (C—H = 0.93–0.97 Å) and refined as riding with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for the methyl group.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: Please give details; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).
(C12H9N2)[SbBr(C12H8N2)4]·CH2Cl2 | Z = 2 |
Mr = 887.73 | F(000) = 844 |
Triclinic, P1 | Dx = 2.019 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.471 (8) Å | Cell parameters from 2399 reflections |
b = 11.582 (9) Å | θ = 2.5–25.3° |
c = 12.154 (9) Å | µ = 6.62 mm−1 |
α = 65.296 (8)° | T = 298 K |
β = 84.535 (9)° | Block, yellow |
γ = 88.244 (9)° | 0.18 × 0.14 × 0.08 mm |
V = 1460.1 (19) Å3 |
Siemens SMART CCD diffractometer | 5056 independent reflections |
Radiation source: fine-focus sealed tube | 3378 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→12 |
Tmin = 0.382, Tmax = 0.619 | k = −12→13 |
7508 measured reflections | l = −11→14 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0567P)2] where P = (Fo2 + 2Fc2)/3 |
5056 reflections | (Δ/σ)max = 0.004 |
319 parameters | Δρmax = 1.81 e Å−3 |
9 restraints | Δρmin = −1.12 e Å−3 |
(C12H9N2)[SbBr(C12H8N2)4]·CH2Cl2 | γ = 88.244 (9)° |
Mr = 887.73 | V = 1460.1 (19) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.471 (8) Å | Mo Kα radiation |
b = 11.582 (9) Å | µ = 6.62 mm−1 |
c = 12.154 (9) Å | T = 298 K |
α = 65.296 (8)° | 0.18 × 0.14 × 0.08 mm |
β = 84.535 (9)° |
Siemens SMART CCD diffractometer | 5056 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3378 reflections with I > 2σ(I) |
Tmin = 0.382, Tmax = 0.619 | Rint = 0.025 |
7508 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 9 restraints |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 1.01 | Δρmax = 1.81 e Å−3 |
5056 reflections | Δρmin = −1.12 e Å−3 |
319 parameters |
x | y | z | Uiso*/Ueq | ||
Sb1 | 0.74351 (4) | 0.63084 (4) | 0.10677 (4) | 0.03882 (16) | |
Br1 | 0.49189 (7) | 0.70645 (7) | 0.05598 (7) | 0.0551 (2) | |
Br2 | 0.77617 (8) | 0.37772 (7) | 0.14655 (8) | 0.0652 (3) | |
Br3 | 0.83075 (7) | 0.73103 (7) | −0.13286 (7) | 0.0577 (2) | |
Br4 | 0.69659 (9) | 0.56828 (8) | 0.35088 (8) | 0.0731 (3) | |
Cl1 | 1.0701 (5) | 0.3451 (6) | 0.5116 (5) | 0.2246 (18) | |
Cl2 | 0.9780 (4) | 0.1461 (6) | 0.4665 (5) | 0.2246 (18) | |
N1 | 0.9366 (4) | 0.6463 (5) | 0.1393 (5) | 0.0398 (14) | |
N2 | 0.7796 (5) | 0.8350 (5) | 0.1013 (5) | 0.0457 (15) | |
N3 | 0.4363 (5) | −0.0210 (6) | 0.2689 (6) | 0.0569 (17) | |
N4 | 0.4445 (5) | 0.2270 (6) | 0.2372 (5) | 0.0500 (16) | |
H4 | 0.4677 | 0.2034 | 0.1804 | 0.060* | |
C1 | 1.0167 (6) | 0.5575 (7) | 0.1477 (7) | 0.0488 (19) | |
H1 | 0.9951 | 0.4868 | 0.1363 | 0.059* | |
C2 | 1.1303 (7) | 0.5663 (8) | 0.1728 (7) | 0.061 (2) | |
H2 | 1.1838 | 0.5025 | 0.1788 | 0.073* | |
C3 | 1.1625 (7) | 0.6716 (9) | 0.1886 (8) | 0.065 (2) | |
H3 | 1.2386 | 0.6791 | 0.2055 | 0.078* | |
C4 | 1.0815 (6) | 0.7671 (7) | 0.1794 (6) | 0.0477 (19) | |
C5 | 0.9690 (6) | 0.7522 (6) | 0.1522 (6) | 0.0397 (17) | |
C6 | 0.8850 (6) | 0.8488 (6) | 0.1358 (6) | 0.0405 (17) | |
C7 | 0.9154 (7) | 0.9599 (6) | 0.1483 (6) | 0.052 (2) | |
C8 | 0.8308 (9) | 1.0549 (7) | 0.1263 (8) | 0.069 (3) | |
H8 | 0.8469 | 1.1290 | 0.1344 | 0.083* | |
C9 | 0.7264 (9) | 1.0383 (7) | 0.0936 (8) | 0.072 (3) | |
H9 | 0.6695 | 1.1006 | 0.0795 | 0.087* | |
C10 | 0.7036 (7) | 0.9268 (7) | 0.0809 (7) | 0.059 (2) | |
H10 | 0.6313 | 0.9174 | 0.0568 | 0.071* | |
C11 | 1.1071 (8) | 0.8766 (8) | 0.1957 (8) | 0.067 (2) | |
H11 | 1.1808 | 0.8848 | 0.2177 | 0.080* | |
C12 | 1.0297 (8) | 0.9689 (8) | 0.1808 (8) | 0.071 (3) | |
H12 | 1.0506 | 1.0401 | 0.1918 | 0.085* | |
C13 | 0.4339 (8) | −0.1411 (8) | 0.2883 (8) | 0.069 (2) | |
H13 | 0.4627 | −0.1633 | 0.2256 | 0.082* | |
C14 | 0.3901 (7) | −0.2374 (8) | 0.3986 (9) | 0.068 (2) | |
H14 | 0.3891 | −0.3211 | 0.4074 | 0.081* | |
C15 | 0.3489 (7) | −0.2098 (8) | 0.4932 (8) | 0.064 (2) | |
H15 | 0.3213 | −0.2738 | 0.5674 | 0.076* | |
C16 | 0.3490 (7) | −0.0823 (7) | 0.4765 (7) | 0.053 (2) | |
C17 | 0.3943 (6) | 0.0078 (6) | 0.3625 (6) | 0.0425 (17) | |
C18 | 0.3990 (6) | 0.1376 (7) | 0.3458 (7) | 0.0456 (18) | |
C19 | 0.3614 (6) | 0.1753 (7) | 0.4382 (7) | 0.0499 (19) | |
C20 | 0.3712 (7) | 0.3039 (8) | 0.4138 (8) | 0.062 (2) | |
H20 | 0.3445 | 0.3316 | 0.4732 | 0.075* | |
C21 | 0.4194 (7) | 0.3887 (8) | 0.3042 (8) | 0.060 (2) | |
H21 | 0.4285 | 0.4734 | 0.2901 | 0.072* | |
C22 | 0.4549 (7) | 0.3494 (7) | 0.2141 (7) | 0.055 (2) | |
H22 | 0.4857 | 0.4076 | 0.1380 | 0.066* | |
C23 | 0.3076 (7) | −0.0432 (8) | 0.5711 (7) | 0.060 (2) | |
H23 | 0.2756 | −0.1032 | 0.6457 | 0.072* | |
C24 | 0.3148 (7) | 0.0804 (8) | 0.5525 (7) | 0.064 (2) | |
H24 | 0.2890 | 0.1037 | 0.6151 | 0.076* | |
C25 | 0.9717 (14) | 0.3019 (13) | 0.4409 (15) | 0.207 (7) | |
H25A | 0.9846 | 0.3534 | 0.3541 | 0.248* | |
H25B | 0.8937 | 0.3197 | 0.4679 | 0.248* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sb1 | 0.0378 (3) | 0.0331 (3) | 0.0476 (3) | 0.0008 (2) | −0.0008 (2) | −0.0195 (2) |
Br1 | 0.0486 (5) | 0.0630 (5) | 0.0542 (5) | 0.0059 (4) | −0.0029 (4) | −0.0257 (4) |
Br2 | 0.0822 (6) | 0.0437 (4) | 0.0748 (6) | −0.0054 (4) | 0.0056 (5) | −0.0319 (4) |
Br3 | 0.0639 (5) | 0.0546 (5) | 0.0564 (5) | −0.0063 (4) | −0.0001 (4) | −0.0256 (4) |
Br4 | 0.1065 (7) | 0.0592 (5) | 0.0570 (5) | −0.0105 (5) | 0.0125 (5) | −0.0310 (4) |
Cl1 | 0.173 (3) | 0.312 (5) | 0.205 (4) | −0.014 (3) | −0.007 (3) | −0.125 (4) |
Cl2 | 0.173 (3) | 0.312 (5) | 0.205 (4) | −0.014 (3) | −0.007 (3) | −0.125 (4) |
N1 | 0.037 (3) | 0.042 (3) | 0.051 (4) | 0.004 (3) | −0.005 (3) | −0.029 (3) |
N2 | 0.044 (4) | 0.032 (3) | 0.056 (4) | 0.005 (3) | 0.009 (3) | −0.016 (3) |
N3 | 0.063 (4) | 0.057 (4) | 0.059 (4) | −0.003 (3) | 0.004 (4) | −0.034 (3) |
N4 | 0.051 (4) | 0.054 (4) | 0.049 (4) | −0.006 (3) | 0.005 (3) | −0.028 (3) |
C1 | 0.049 (5) | 0.052 (4) | 0.059 (5) | 0.011 (4) | −0.013 (4) | −0.035 (4) |
C2 | 0.046 (5) | 0.071 (6) | 0.079 (6) | 0.021 (4) | −0.015 (4) | −0.043 (5) |
C3 | 0.031 (4) | 0.091 (7) | 0.076 (6) | 0.001 (4) | −0.004 (4) | −0.038 (5) |
C4 | 0.043 (5) | 0.059 (5) | 0.044 (4) | −0.010 (4) | −0.002 (4) | −0.024 (4) |
C5 | 0.044 (4) | 0.037 (4) | 0.036 (4) | −0.002 (3) | 0.004 (3) | −0.015 (3) |
C6 | 0.044 (4) | 0.038 (4) | 0.041 (4) | −0.003 (3) | 0.009 (3) | −0.020 (3) |
C7 | 0.069 (6) | 0.036 (4) | 0.046 (5) | −0.012 (4) | 0.017 (4) | −0.018 (3) |
C8 | 0.105 (8) | 0.034 (4) | 0.064 (6) | −0.011 (5) | 0.029 (6) | −0.024 (4) |
C9 | 0.088 (7) | 0.033 (4) | 0.081 (7) | 0.011 (5) | 0.018 (6) | −0.015 (4) |
C10 | 0.044 (5) | 0.040 (4) | 0.076 (6) | 0.005 (4) | 0.010 (4) | −0.010 (4) |
C11 | 0.063 (6) | 0.071 (6) | 0.070 (6) | −0.020 (5) | −0.011 (5) | −0.030 (5) |
C12 | 0.085 (7) | 0.056 (5) | 0.081 (7) | −0.027 (5) | 0.008 (6) | −0.040 (5) |
C13 | 0.077 (6) | 0.068 (6) | 0.077 (6) | 0.004 (5) | −0.005 (5) | −0.046 (5) |
C14 | 0.071 (6) | 0.051 (5) | 0.084 (7) | −0.002 (4) | −0.002 (5) | −0.032 (5) |
C15 | 0.069 (6) | 0.052 (5) | 0.057 (5) | −0.003 (4) | −0.010 (5) | −0.009 (4) |
C16 | 0.054 (5) | 0.055 (5) | 0.047 (5) | −0.002 (4) | 0.000 (4) | −0.020 (4) |
C17 | 0.039 (4) | 0.044 (4) | 0.044 (4) | 0.001 (3) | −0.001 (4) | −0.018 (4) |
C18 | 0.042 (4) | 0.049 (4) | 0.046 (5) | 0.006 (4) | −0.004 (4) | −0.022 (4) |
C19 | 0.046 (5) | 0.059 (5) | 0.050 (5) | 0.002 (4) | −0.001 (4) | −0.029 (4) |
C20 | 0.076 (6) | 0.066 (6) | 0.060 (6) | 0.014 (5) | −0.010 (5) | −0.042 (5) |
C21 | 0.066 (6) | 0.051 (5) | 0.072 (6) | −0.001 (4) | −0.010 (5) | −0.033 (5) |
C22 | 0.055 (5) | 0.047 (5) | 0.059 (5) | −0.001 (4) | −0.007 (4) | −0.017 (4) |
C23 | 0.064 (5) | 0.058 (5) | 0.041 (5) | −0.009 (4) | 0.009 (4) | −0.008 (4) |
C24 | 0.072 (6) | 0.075 (6) | 0.046 (5) | 0.005 (5) | 0.007 (4) | −0.029 (5) |
C25 | 0.173 (10) | 0.174 (10) | 0.200 (10) | −0.040 (8) | −0.051 (8) | 0.004 (8) |
Sb1—N1 | 2.312 (5) | C8—H8 | 0.9300 |
Sb1—N2 | 2.386 (6) | C9—C10 | 1.399 (11) |
Sb1—Br3 | 2.742 (2) | C9—H9 | 0.9300 |
Sb1—Br4 | 2.746 (2) | C10—H10 | 0.9300 |
Sb1—Br2 | 2.784 (2) | C11—C12 | 1.332 (11) |
Sb1—Br1 | 3.035 (2) | C11—H11 | 0.9300 |
Cl1—C25 | 1.686 (13) | C12—H12 | 0.9300 |
Cl2—C25 | 1.698 (13) | C13—C14 | 1.396 (11) |
N1—C1 | 1.336 (8) | C13—H13 | 0.9300 |
N1—C5 | 1.366 (8) | C14—C15 | 1.357 (11) |
N2—C10 | 1.310 (8) | C14—H14 | 0.9300 |
N2—C6 | 1.352 (8) | C15—C16 | 1.403 (10) |
N3—C13 | 1.311 (10) | C15—H15 | 0.9300 |
N3—C17 | 1.356 (8) | C16—C17 | 1.402 (10) |
N4—C22 | 1.332 (9) | C16—C23 | 1.440 (10) |
N4—C18 | 1.359 (9) | C17—C18 | 1.433 (10) |
N4—H4 | 0.8600 | C18—C19 | 1.394 (9) |
C1—C2 | 1.382 (10) | C19—C20 | 1.397 (10) |
C1—H1 | 0.9300 | C19—C24 | 1.429 (10) |
C2—C3 | 1.378 (11) | C20—C21 | 1.358 (11) |
C2—H2 | 0.9300 | C20—H20 | 0.9300 |
C3—C4 | 1.398 (10) | C21—C22 | 1.376 (10) |
C3—H3 | 0.9300 | C21—H21 | 0.9300 |
C4—C5 | 1.395 (9) | C22—H22 | 0.9300 |
C4—C11 | 1.406 (10) | C23—C24 | 1.356 (11) |
C5—C6 | 1.416 (9) | C23—H23 | 0.9300 |
C6—C7 | 1.414 (9) | C24—H24 | 0.9300 |
C7—C8 | 1.400 (11) | C25—H25A | 0.9700 |
C7—C12 | 1.425 (11) | C25—H25B | 0.9700 |
C8—C9 | 1.340 (12) | ||
N1—Sb1—N2 | 70.23 (19) | N2—C10—C9 | 123.0 (8) |
N1—Sb1—Br3 | 83.16 (14) | N2—C10—H10 | 118.5 |
N2—Sb1—Br3 | 86.42 (14) | C9—C10—H10 | 118.5 |
N1—Sb1—Br4 | 85.43 (14) | C12—C11—C4 | 122.5 (8) |
N2—Sb1—Br4 | 82.19 (14) | C12—C11—H11 | 118.8 |
Br3—Sb1—Br4 | 166.06 (3) | C4—C11—H11 | 118.8 |
N1—Sb1—Br2 | 90.30 (13) | C11—C12—C7 | 120.8 (7) |
N2—Sb1—Br2 | 160.06 (15) | C11—C12—H12 | 119.6 |
Br3—Sb1—Br2 | 95.76 (3) | C7—C12—H12 | 119.6 |
Br4—Sb1—Br2 | 92.28 (3) | N3—C13—C14 | 123.1 (8) |
N1—Sb1—Br1 | 159.61 (13) | N3—C13—H13 | 118.5 |
N2—Sb1—Br1 | 89.39 (15) | C14—C13—H13 | 118.5 |
Br3—Sb1—Br1 | 95.34 (4) | C15—C14—C13 | 120.5 (8) |
Br4—Sb1—Br1 | 92.57 (4) | C15—C14—H14 | 119.8 |
Br2—Sb1—Br1 | 110.07 (3) | C13—C14—H14 | 119.8 |
C1—N1—C5 | 118.8 (6) | C14—C15—C16 | 118.5 (7) |
C1—N1—Sb1 | 123.8 (4) | C14—C15—H15 | 120.8 |
C5—N1—Sb1 | 117.3 (4) | C16—C15—H15 | 120.8 |
C10—N2—C6 | 118.6 (6) | C17—C16—C15 | 117.0 (7) |
C10—N2—Sb1 | 126.1 (5) | C17—C16—C23 | 120.3 (7) |
C6—N2—Sb1 | 114.9 (4) | C15—C16—C23 | 122.8 (7) |
C13—N3—C17 | 116.9 (7) | N3—C17—C16 | 124.1 (7) |
C22—N4—C18 | 123.4 (6) | N3—C17—C18 | 118.4 (6) |
C22—N4—H4 | 118.3 | C16—C17—C18 | 117.5 (6) |
C18—N4—H4 | 118.3 | N4—C18—C19 | 118.6 (7) |
N1—C1—C2 | 122.7 (7) | N4—C18—C17 | 119.1 (6) |
N1—C1—H1 | 118.7 | C19—C18—C17 | 122.3 (7) |
C2—C1—H1 | 118.7 | C18—C19—C20 | 118.1 (7) |
C3—C2—C1 | 118.7 (7) | C18—C19—C24 | 118.2 (7) |
C3—C2—H2 | 120.7 | C20—C19—C24 | 123.6 (7) |
C1—C2—H2 | 120.7 | C21—C20—C19 | 120.7 (7) |
C2—C3—C4 | 120.3 (7) | C21—C20—H20 | 119.7 |
C2—C3—H3 | 119.8 | C19—C20—H20 | 119.7 |
C4—C3—H3 | 119.8 | C20—C21—C22 | 120.0 (7) |
C5—C4—C3 | 117.7 (7) | C20—C21—H21 | 120.0 |
C5—C4—C11 | 118.6 (7) | C22—C21—H21 | 120.0 |
C3—C4—C11 | 123.8 (7) | N4—C22—C21 | 119.1 (7) |
N1—C5—C4 | 121.8 (6) | N4—C22—H22 | 120.4 |
N1—C5—C6 | 118.1 (6) | C21—C22—H22 | 120.4 |
C4—C5—C6 | 120.1 (6) | C24—C23—C16 | 120.6 (7) |
N2—C6—C7 | 121.8 (6) | C24—C23—H23 | 119.7 |
N2—C6—C5 | 118.4 (6) | C16—C23—H23 | 119.7 |
C7—C6—C5 | 119.7 (7) | C23—C24—C19 | 121.1 (7) |
C8—C7—C6 | 117.5 (8) | C23—C24—H24 | 119.4 |
C8—C7—C12 | 124.2 (8) | C19—C24—H24 | 119.4 |
C6—C7—C12 | 118.3 (7) | Cl1—C25—Cl2 | 113.9 (9) |
C9—C8—C7 | 119.6 (8) | Cl1—C25—H25A | 108.8 |
C9—C8—H8 | 120.2 | Cl2—C25—H25A | 108.8 |
C7—C8—H8 | 120.2 | Cl1—C25—H25B | 108.8 |
C8—C9—C10 | 119.6 (8) | Cl2—C25—H25B | 108.8 |
C8—C9—H9 | 120.2 | H25A—C25—H25B | 107.7 |
C10—C9—H9 | 120.2 |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4···Br1i | 0.86 | 2.61 | 3.327 (6) | 141 |
Symmetry code: (i) −x+1, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | (C12H9N2)[SbBr(C12H8N2)4]·CH2Cl2 |
Mr | 887.73 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 11.471 (8), 11.582 (9), 12.154 (9) |
α, β, γ (°) | 65.296 (8), 84.535 (9), 88.244 (9) |
V (Å3) | 1460.1 (19) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 6.62 |
Crystal size (mm) | 0.18 × 0.14 × 0.08 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.382, 0.619 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7508, 5056, 3378 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.112, 1.01 |
No. of reflections | 5056 |
No. of parameters | 319 |
No. of restraints | 9 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.81, −1.12 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), Please give details, SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b).
Sb1—N1 | 2.312 (5) | Sb1—Br4 | 2.746 (2) |
Sb1—N2 | 2.386 (6) | Sb1—Br2 | 2.784 (2) |
Sb1—Br3 | 2.742 (2) | Sb1—Br1 | 3.035 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4···Br1i | 0.86 | 2.61 | 3.327 (6) | 141 |
Symmetry code: (i) −x+1, −y+1, −z. |
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The adducts of SbF3 with bi-and tri-dentate nitrogen donors such as 1,10-phenanthroline have been reported (Bertazzi et al., 1983). As a continuation of this work, we report here the synthesis and crystal structure of the title compound, (I), (Fig. 1). In this complex, the antimony atom is six-coordinated by two N atoms of phen and four Br atoms with a distorted cis-SbN2Br4 octahedral geometry (Table 1).
The charge on the anion is balanced by a phenanthrolinium cation, which bonds to the anion via an N—H···Br hydrongen bond (Table 2, Fig. 2). A dichloromethane solvent molecule completes the structure.