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The title compound, [Sb2(C6H5)4(C5H8Cl2)], is the product of a substitution reaction of 2,2-bis(chloromethyl)-1,3-dichloropropane with sodium diphenylstibide. Adjacent phenyl groups embrace each other in a parallel fashion in order to minimize interaction. The molecule has crystallographic twofold rotation symmetry.
Supporting information
CCDC reference: 170286
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.004 Å
- R factor = 0.025
- wR factor = 0.063
- Data-to-parameter ratio = 18.1
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
General Notes
ABSTY_01 Extra text has been found in the _exptl_absorpt_correction_type
field, which should be only a single keyword. A literature
citation should be included in the _exptl_absorpt_process_details
field.
Cell refinement: DENZO (Hooft, 1998) and COLLECT (Otwinowski & Minor, 1997); data reduction: DENZO and COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1990).
Crystal data top
[Sb2(C6H5)4(C5H8Cl2)] | F(000) = 1352 |
Mr = 690.91 | Dx = 1.702 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 14.578 (3) Å | Cell parameters from 6922 reflections |
b = 12.009 (2) Å | θ = 2.9–26.4° |
c = 15.849 (3) Å | µ = 2.22 mm−1 |
β = 103.67 (3)° | T = 150 K |
V = 2696.2 (9) Å3 | Needle, colourless |
Z = 4 | 0.22 × 0.08 × 0.06 mm |
Data collection top
Nonius KappaCCD area-detector diffractometer | 2458 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.058 |
Absorption correction: multi-scans (SORTAV; Blessing, 1997) | θmax = 26.4°, θmin = 3.2° |
Tmin = 0.641, Tmax = 0.878 | h = −18→17 |
9556 measured reflections | k = −14→14 |
2739 independent reflections | l = −18→19 |
Refinement top
Refinement on F2 | H-atom parameters constrained |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0253P)2 + 1.756P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.026 | (Δ/σ)max = 0.001 |
wR(F2) = 0.063 | Δρmax = 0.77 e Å−3 |
S = 1.07 | Δρmin = −0.70 e Å−3 |
2739 reflections | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
151 parameters | Extinction coefficient: 0.00078 (11) |
0 restraints | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1 | 0.19743 (18) | 0.9803 (2) | 0.09451 (16) | 0.0229 (5) | |
C2 | 0.24796 (18) | 0.8963 (2) | 0.06461 (18) | 0.0285 (6) | |
H2 | 0.2556 | 0.8263 | 0.0933 | 0.034* | |
C3 | 0.28708 (19) | 0.9129 (2) | −0.00580 (19) | 0.0329 (6) | |
H3 | 0.3217 | 0.8549 | −0.0247 | 0.039* | |
C4 | 0.27586 (19) | 1.0136 (3) | −0.04866 (19) | 0.0323 (6) | |
H4 | 0.3029 | 1.0253 | −0.0969 | 0.039* | |
C5 | 0.22453 (19) | 1.0983 (2) | −0.02071 (18) | 0.0322 (6) | |
H5 | 0.2151 | 1.1673 | −0.0508 | 0.039* | |
C6 | 0.18742 (19) | 1.0814 (2) | 0.05103 (18) | 0.0297 (6) | |
H6 | 0.1544 | 1.1403 | 0.0709 | 0.036* | |
C7 | 0.08813 (18) | 0.7910 (2) | 0.16749 (17) | 0.0265 (6) | |
C8 | 0.02188 (19) | 0.7794 (2) | 0.08824 (18) | 0.0340 (6) | |
H8 | 0.0029 | 0.8427 | 0.0525 | 0.041* | |
C9 | −0.0162 (2) | 0.6758 (2) | 0.0616 (2) | 0.0424 (8) | |
H9 | −0.0616 | 0.6687 | 0.0079 | 0.051* | |
C10 | 0.0114 (2) | 0.5832 (3) | 0.1127 (2) | 0.0448 (8) | |
H10 | −0.0149 | 0.5124 | 0.0944 | 0.054* | |
C11 | 0.0774 (2) | 0.5938 (2) | 0.1907 (2) | 0.0429 (8) | |
H11 | 0.0969 | 0.53 | 0.2258 | 0.052* | |
C12 | 0.11514 (19) | 0.6970 (2) | 0.21784 (19) | 0.0316 (6) | |
H12 | 0.1602 | 0.7036 | 0.2718 | 0.038* | |
C13 | 0.01975 (18) | 1.04800 (18) | 0.17578 (17) | 0.0199 (5) | |
H13A | 0.0232 | 1.0971 | 0.1265 | 0.024* | |
H13B | −0.0342 | 0.9967 | 0.1557 | 0.024* | |
C14 | 0 | 1.1206 (3) | 0.25 | 0.0190 (7) | |
C15 | 0.08448 (17) | 1.1935 (2) | 0.29216 (16) | 0.0239 (5) | |
H15A | 0.1375 | 1.1449 | 0.321 | 0.029* | |
H15B | 0.0672 | 1.2402 | 0.3374 | 0.029* | |
Sb1 | 0.149395 (11) | 0.949625 (13) | 0.210673 (10) | 0.02181 (10) | |
Cl1 | 0.12339 (5) | 1.28256 (6) | 0.21571 (5) | 0.03507 (18) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0176 (12) | 0.0260 (13) | 0.0250 (13) | −0.0020 (10) | 0.0049 (10) | −0.0041 (11) |
C2 | 0.0244 (13) | 0.0252 (14) | 0.0365 (15) | 0.0044 (11) | 0.0081 (12) | −0.0011 (12) |
C3 | 0.0263 (15) | 0.0337 (15) | 0.0392 (16) | 0.0041 (12) | 0.0090 (13) | −0.0098 (13) |
C4 | 0.0252 (15) | 0.0411 (16) | 0.0320 (15) | −0.0011 (13) | 0.0092 (12) | −0.0037 (13) |
C5 | 0.0308 (15) | 0.0310 (15) | 0.0366 (15) | 0.0002 (12) | 0.0114 (13) | 0.0044 (12) |
C6 | 0.0285 (15) | 0.0231 (13) | 0.0385 (16) | 0.0020 (11) | 0.0100 (13) | −0.0011 (12) |
C7 | 0.0241 (13) | 0.0200 (13) | 0.0390 (15) | 0.0018 (10) | 0.0147 (12) | −0.0002 (11) |
C8 | 0.0304 (15) | 0.0283 (15) | 0.0423 (16) | 0.0011 (12) | 0.0069 (13) | −0.0041 (12) |
C9 | 0.0301 (16) | 0.0377 (18) | 0.058 (2) | −0.0054 (13) | 0.0078 (14) | −0.0160 (15) |
C10 | 0.0407 (18) | 0.0274 (16) | 0.075 (2) | −0.0087 (14) | 0.0311 (18) | −0.0164 (17) |
C11 | 0.052 (2) | 0.0192 (14) | 0.070 (2) | 0.0084 (14) | 0.0386 (18) | 0.0093 (15) |
C12 | 0.0300 (15) | 0.0239 (14) | 0.0449 (17) | 0.0034 (12) | 0.0170 (13) | 0.0023 (12) |
C13 | 0.0146 (12) | 0.0185 (13) | 0.0256 (13) | −0.0002 (9) | 0.0026 (11) | −0.0014 (9) |
C14 | 0.0157 (16) | 0.0149 (16) | 0.0265 (18) | 0 | 0.0050 (14) | 0 |
C15 | 0.0221 (12) | 0.0193 (12) | 0.0317 (14) | −0.0017 (10) | 0.0089 (11) | 0.0001 (10) |
Sb1 | 0.01911 (13) | 0.01996 (13) | 0.02567 (14) | 0.00323 (6) | 0.00394 (9) | −0.00063 (6) |
Cl1 | 0.0350 (4) | 0.0252 (4) | 0.0477 (4) | −0.0108 (3) | 0.0151 (3) | 0.0010 (3) |
Geometric parameters (Å, º) top
C1—C6 | 1.386 (4) | C8—C9 | 1.386 (4) |
C1—C2 | 1.396 (4) | C9—C10 | 1.379 (5) |
C1—Sb1 | 2.151 (3) | C10—C11 | 1.381 (5) |
C2—C3 | 1.383 (4) | C11—C12 | 1.383 (4) |
C3—C4 | 1.378 (4) | C13—C14 | 1.545 (3) |
C4—C5 | 1.395 (4) | C13—Sb1 | 2.186 (2) |
C5—C6 | 1.385 (4) | C14—C15 | 1.530 (3) |
C7—C12 | 1.384 (4) | C14—C15i | 1.530 (3) |
C7—C8 | 1.399 (4) | C14—C13i | 1.545 (3) |
C7—Sb1 | 2.146 (3) | C15—Cl1 | 1.805 (2) |
| | | |
C6—C1—C2 | 117.8 (2) | C10—C11—C12 | 120.2 (3) |
C6—C1—Sb1 | 123.94 (19) | C11—C12—C7 | 120.9 (3) |
C2—C1—Sb1 | 118.1 (2) | C14—C13—Sb1 | 114.70 (15) |
C3—C2—C1 | 121.4 (3) | C15—C14—C15i | 110.2 (3) |
C4—C3—C2 | 120.1 (3) | C15—C14—C13i | 105.43 (13) |
C3—C4—C5 | 119.5 (3) | C15i—C14—C13i | 112.31 (13) |
C6—C5—C4 | 119.8 (3) | C15—C14—C13 | 112.31 (13) |
C5—C6—C1 | 121.4 (3) | C15i—C14—C13 | 105.43 (13) |
C12—C7—C8 | 118.6 (2) | C13i—C14—C13 | 111.3 (3) |
C12—C7—Sb1 | 120.0 (2) | C14—C15—Cl1 | 113.22 (15) |
C8—C7—Sb1 | 121.45 (19) | C7—Sb1—C1 | 94.27 (10) |
C9—C8—C7 | 120.3 (3) | C7—Sb1—C13 | 97.43 (9) |
C10—C9—C8 | 120.3 (3) | C1—Sb1—C13 | 97.34 (10) |
C9—C10—C11 | 119.7 (3) | | |
Symmetry code: (i) −x, y, −z+1/2. |
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