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metal-organic compounds
catena-Poly[dimethylphenyltin(IV)-μ-trifluoroacetato-O:O′], [(CH3)2(C6H5)SnOC(O)CF3]n, adopts a helical carboxylate-bridged chain structure, in which the Sn atom shows trans-C3SnO2 trigonal–bipyramidal coordination, with unequal Sn—O distances of 2.181 (2) and 2.580 (2) Å.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802018779/ya6139sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802018779/ya6139Isup2.hkl |
CCDC reference: 200731
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.020
- wR factor = 0.051
- Data-to-parameter ratio = 14.1
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level A:
TYPE_089 Alert A _refine_ls_abs_structure_Flack is not of type numb. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C10 H11 F3 O2 Sn1 Atom count from _chemical_formula_moiety: REFLT_03 From the CIF: _diffrn_reflns_theta_max 26.00 From the CIF: _reflns_number_total 2465 Count of symmetry unique reflns 1443 Completeness (_total/calc) 170.82% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1022 Fraction of Friedel pairs measured 0.708 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check
Computing details top
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-II (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly(dimethylphenyltin-µ-trifluoroacetato-O;O') top
Crystal data top
[Sn(C6H5)(C2F3O2)(CH3)2] | Dx = 1.801 Mg m−3 |
Mr = 338.88 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 5881 reflections |
a = 6.6552 (3) Å | θ = 2.2–26.0° |
b = 10.9949 (5) Å | µ = 2.07 mm−1 |
c = 17.0794 (7) Å | T = 293 K |
V = 1249.8 (1) Å3 | Prism, colorless |
Z = 4 | 0.24 × 0.16 × 0.05 mm |
F(000) = 656 |
Data collection top
Bruker AXS CCD area-detector diffractometer | 2465 independent reflections |
Radiation source: rotating anode tube | 2364 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
ω scan | θmax = 26.0°, θmin = 2.2° |
Absorption correction: multi-scan SADABS (Sheldrick, 1996) | h = −8→8 |
Tmin = 0.637, Tmax = 0.904 | k = −13→13 |
10949 measured reflections | l = −21→21 |
Refinement top
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)] = 0.020 | H-atom parameters constrained |
wR(F2) = 0.051 | w = 1/[σ2(Fo2) + (0.0355P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.99 | (Δ/σ)max < 0.001 |
2465 reflections | Δρmax = 0.27 e Å−3 |
175 parameters | Δρmin = −0.43 e Å−3 |
66 restraints | Absolute structure: Flack & Schwarzenbach (1988) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.04 (3); 1197 Friedel pairs were measured |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sn1 | 0.46474 (4) | 0.64930 (2) | 0.78525 (1) | 0.0493 (1) | |
F1 | 0.284 (2) | 0.2015 (5) | 0.8995 (7) | 0.119 (3) | 0.61 (2) |
F2 | 0.278 (2) | 0.3519 (8) | 0.9762 (3) | 0.105 (3) | 0.61 (2) |
F3 | 0.0448 (9) | 0.329 (1) | 0.8952 (8) | 0.121 (3) | 0.61 (2) |
F1' | 0.212 (2) | 0.2033 (8) | 0.881 (1) | 0.085 (4) | 0.39 (2) |
F2' | 0.362 (3) | 0.316 (2) | 0.964 (1) | 0.134 (6) | 0.39 (2) |
F3' | 0.065 (2) | 0.355 (1) | 0.926 (1) | 0.111 (5) | 0.39 (2) |
O1 | 0.3368 (5) | 0.5046 (2) | 0.8569 (2) | 0.068 (1) | |
O2 | 0.4165 (6) | 0.3442 (2) | 0.7851 (2) | 0.083 (1) | |
C1 | 0.2897 (8) | 0.6128 (5) | 0.6858 (2) | 0.080 (1) | |
C2 | 0.7652 (6) | 0.5886 (4) | 0.7920 (3) | 0.073 (1) | |
C3 | 0.3741 (6) | 0.7798 (3) | 0.8689 (2) | 0.050 (1) | |
C4 | 0.1841 (6) | 0.8335 (3) | 0.8663 (2) | 0.064 (1) | |
C5 | 0.1328 (8) | 0.9195 (4) | 0.9239 (3) | 0.076 (1) | |
C6 | 0.2621 (9) | 0.9501 (4) | 0.9805 (2) | 0.079 (1) | |
C7 | 0.4484 (9) | 0.8989 (4) | 0.9834 (2) | 0.075 (1) | |
C8 | 0.5032 (7) | 0.8133 (3) | 0.9279 (2) | 0.065 (1) | |
C9 | 0.3444 (6) | 0.3933 (3) | 0.8420 (2) | 0.058 (1) | |
C10 | 0.2403 (7) | 0.3165 (3) | 0.9045 (2) | 0.079 (1) | |
H1a | 0.2390 | 0.6878 | 0.6648 | 0.120* | |
H1b | 0.1792 | 0.5612 | 0.7000 | 0.120* | |
H1c | 0.3707 | 0.5728 | 0.6471 | 0.120* | |
H2a | 0.7921 | 0.5592 | 0.8439 | 0.110* | |
H2b | 0.8542 | 0.6549 | 0.7803 | 0.110* | |
H2c | 0.7859 | 0.5242 | 0.7549 | 0.110* | |
H4 | 0.0931 | 0.8128 | 0.8272 | 0.077* | |
H5 | 0.0065 | 0.9556 | 0.9227 | 0.091* | |
H6 | 0.2247 | 1.0069 | 1.0181 | 0.095* | |
H7 | 0.5383 | 0.9212 | 1.0225 | 0.090* | |
H8 | 0.6298 | 0.7777 | 0.9306 | 0.077* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.0616 (1) | 0.0368 (1) | 0.0495 (1) | −0.0023 (1) | 0.0071 (1) | −0.0046 (1) |
F1 | 0.198 (8) | 0.043 (3) | 0.114 (6) | 0.000 (4) | 0.052 (6) | 0.017 (3) |
F2 | 0.170 (7) | 0.091 (4) | 0.052 (3) | −0.010 (4) | 0.025 (3) | 0.008 (2) |
F3 | 0.118 (5) | 0.120 (6) | 0.125 (6) | −0.049 (4) | 0.031 (4) | −0.001 (4) |
F1' | 0.121 (7) | 0.044 (4) | 0.090 (6) | −0.015 (4) | 0.019 (5) | 0.009 (4) |
F2' | 0.17 (1) | 0.139 (9) | 0.097 (7) | −0.023 (7) | −0.008 (7) | 0.035 (6) |
F3' | 0.141 (8) | 0.073 (5) | 0.118 (8) | 0.009 (6) | 0.084 (6) | −0.006 (5) |
O1 | 0.103 (2) | 0.035 (1) | 0.067 (1) | −0.009 (1) | 0.026 (2) | −0.002 (1) |
O2 | 0.130 (2) | 0.043 (1) | 0.077 (2) | 0.003 (2) | 0.041 (2) | −0.007 (1) |
C1 | 0.078 (3) | 0.096 (3) | 0.065 (2) | −0.008 (2) | −0.006 (2) | −0.008 (2) |
C2 | 0.065 (2) | 0.076 (2) | 0.079 (3) | 0.008 (2) | 0.005 (2) | −0.001 (2) |
C3 | 0.070 (2) | 0.030 (1) | 0.049 (2) | −0.002 (1) | 0.009 (2) | 0.006 (1) |
C4 | 0.072 (2) | 0.055 (2) | 0.064 (2) | 0.005 (2) | 0.000 (2) | 0.001 (2) |
C5 | 0.094 (3) | 0.058 (2) | 0.074 (3) | 0.022 (2) | 0.019 (3) | 0.005 (2) |
C6 | 0.136 (4) | 0.049 (2) | 0.053 (2) | 0.012 (3) | 0.017 (3) | −0.003 (2) |
C7 | 0.114 (3) | 0.059 (2) | 0.053 (2) | −0.001 (2) | −0.005 (2) | −0.008 (2) |
C8 | 0.084 (3) | 0.048 (2) | 0.061 (2) | 0.002 (2) | −0.002 (2) | −0.003 (2) |
C9 | 0.080 (2) | 0.037 (1) | 0.055 (2) | −0.002 (2) | 0.015 (2) | −0.003 (1) |
C10 | 0.118 (4) | 0.046 (2) | 0.074 (3) | −0.013 (2) | 0.025 (3) | 0.003 (2) |
Geometric parameters (Å, º) top
Sn1—O1 | 2.181 (2) | C5—C6 | 1.337 (7) |
Sn1—O2i | 2.580 (2) | C6—C7 | 1.363 (7) |
Sn1—C1 | 2.099 (4) | C7—C8 | 1.384 (5) |
Sn1—C2 | 2.111 (4) | C9—C10 | 1.526 (5) |
Sn1—C3 | 2.113 (3) | C1—H1a | 0.9600 |
F1—C10 | 1.300 (6) | C1—H1b | 0.9600 |
F2—C10 | 1.310 (6) | C1—H1c | 0.9600 |
F3—C10 | 1.318 (7) | C2—H2a | 0.9600 |
F1'—C10 | 1.322 (7) | C2—H2b | 0.9600 |
F2'—C10 | 1.298 (7) | C2—H2c | 0.9600 |
F3'—C10 | 1.291 (7) | C4—H4 | 0.9300 |
O1—C9 | 1.250 (4) | C5—H5 | 0.9300 |
O2—C9 | 1.212 (4) | C6—H6 | 0.9300 |
C3—C8 | 1.375 (5) | C7—H7 | 0.9300 |
C3—C4 | 1.396 (6) | C8—H8 | 0.9300 |
C4—C5 | 1.407 (6) | ||
O1—Sn1—O2i | 170.7 (1) | F1'—C10—C9 | 111.8 (8) |
C1—Sn1—O1 | 95.6 (2) | F2'—C10—C9 | 105.5 (8) |
C1—Sn1—O2i | 87.2 (2) | F3'—C10—C9 | 115.0 (7) |
C2—Sn1—O1 | 96.2 (2) | F1—C10—C9 | 113.1 (6) |
C2—Sn1—O2i | 89.9 (2) | F2—C10—C9 | 113.7 (4) |
C3—Sn1—O1 | 90.3 (1) | F3—C10—C9 | 107.8 (5) |
C3—Sn1—O2i | 80.7 (1) | Sn1—C1—H1a | 109.5 |
C1—Sn1—C2 | 120.6 (2) | Sn1—C1—H1b | 109.5 |
C1—Sn1—C3 | 121.2 (2) | H1a—C1—H1b | 109.5 |
C2—Sn1—C3 | 116.6 (2) | Sn1—C1—H1c | 109.5 |
C9—O1—Sn1 | 125.7 (2) | H1a—C1—H1c | 109.5 |
C8—C3—C4 | 118.4 (3) | H1b—C1—H1c | 109.5 |
C8—C3—Sn1 | 119.9 (3) | Sn1—C2—H2a | 109.5 |
C4—C3—Sn1 | 121.6 (3) | Sn1—C2—H2b | 109.5 |
C3—C4—C5 | 118.8 (4) | H2a—C2—H2b | 109.5 |
C6—C5—C4 | 121.2 (4) | Sn1—C2—H2c | 109.5 |
C5—C6—C7 | 120.6 (4) | H2a—C2—H2c | 109.5 |
C6—C7—C8 | 119.7 (4) | H2b—C2—H2c | 109.5 |
C3—C8—C7 | 121.3 (4) | C3—C4—H4 | 120.6 |
O2—C9—O1 | 128.0 (3) | C5—C4—H4 | 120.6 |
O2—C9—C10 | 119.6 (3) | C6—C5—H5 | 119.4 |
O1—C9—C10 | 112.4 (3) | C4—C5—H5 | 119.4 |
F1'—C10—F2' | 108.6 (7) | C5—C6—H6 | 119.7 |
F1'—C10—F3' | 105.4 (7) | C7—C6—H6 | 119.7 |
F2'—C10—F3' | 110.4 (7) | C6—C7—H7 | 120.2 |
F1—C10—F2 | 107.9 (5) | C8—C7—H7 | 120.2 |
F2—C10—F3 | 105.7 (5) | C3—C8—H8 | 119.4 |
F1—C10—F3 | 108.3 (6) | C7—C8—H8 | 119.4 |
C1—Sn1—O1—C9 | 61.4 (4) | Sn1—C3—C8—C7 | 179.8 (3) |
C2—Sn1—O1—C9 | −60.3 (4) | C6—C7—C8—C3 | 0.9 (6) |
C3—Sn1—O1—C9 | −177.2 (4) | Sn1—O1—C9—O2 | −2.6 (7) |
C1—Sn1—C3—C8 | −171.6 (3) | Sn1—O1—C9—C10 | 179.8 (3) |
C2—Sn1—C3—C8 | −5.4 (3) | O2—C9—C10—F3' | −131 (1) |
O1—Sn1—C3—C8 | 91.7 (3) | O1—C9—C10—F3' | 47 (1) |
O2i—Sn1—C3—C8 | −90.6 (3) | O2—C9—C10—F2' | 107 (1) |
C1—Sn1—C3—C4 | 8.8 (3) | O1—C9—C10—F2' | −75 (1) |
C2—Sn1—C3—C4 | 174.9 (3) | O2—C9—C10—F1 | 16 (1) |
O1—Sn1—C3—C4 | −88.0 (3) | O1—C9—C10—F1 | −165.8 (9) |
O2i—Sn1—C3—C4 | 89.7 (3) | O2—C9—C10—F2 | 139.8 (8) |
C8—C3—C4—C5 | 0.1 (5) | O1—C9—C10—F2 | −42.4 (8) |
Sn1—C3—C4—C5 | 179.8 (3) | O2—C9—C10—F3 | −103.3 (8) |
C3—C4—C5—C6 | 0.0 (6) | O1—C9—C10—F3 | 74.5 (8) |
C4—C5—C6—C7 | 0.3 (7) | O2—C9—C10—F1' | −11 (1) |
C5—C6—C7—C8 | −0.7 (7) | O1—C9—C10—F1' | 166.9 (9) |
C4—C3—C8—C7 | −0.5 (5) |
Symmetry code: (i) −x+1, y+1/2, −z+3/2. |
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