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In an attempt to synthesize 1,4-dimethylpyridinium dodecatungstophosphate and 1,4-dimethylpyridinium dodecamolybdophosphate, the title compound, C7H10N+·I3-, was obtained as a by-product. The crystal structure contains a disordered 1,4-dimethylpyridinium cation and a triiodide anion.
Supporting information
CCDC reference: 269891
Key indicators
- Single-crystal X-ray study
- T = 288 K
- Mean (C-C) = 0.013 Å
Some non-H atoms missing
- Disorder in main residue
- R factor = 0.044
- wR factor = 0.105
- Data-to-parameter ratio = 25.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ?
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C4
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1
PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc.
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C7 H10 I3 N1
Atom count from the _atom_site data: C6.64 H10 I3 N1.36
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: Large difference may be due to a
symmetry error - see SYMMG tests
From the CIF: _cell_formula_units_Z 1
From the CIF: _chemical_formula_sum C7 H10 I3 N1
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 7.00 6.64 0.36
H 10.00 10.00 0.00
I 3.00 3.00 0.00
N 1.00 1.36 -0.36
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
4 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
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXL97.
1,4-Dimethylpyridinium triiodide
top
Crystal data top
C7H10N+·I3− | Z = 1 |
Mr = 488.86 | F(000) = 218.3 |
Triclinic, P1 | Dx = 2.525 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 5.469 (2) Å | Cell parameters from 380 reflections |
b = 7.786 (3) Å | θ = 7.5–27.0° |
c = 8.463 (3) Å | µ = 7.24 mm−1 |
α = 108.604 (5)° | T = 288 K |
β = 92.357 (6)° | Needle, brown |
γ = 107.546 (5)° | 0.36 × 0.18 × 0.08 mm |
V = 321.9 (2) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1346 independent reflections |
Radiation source: fine-focus sealed tube | 925 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
φ and ω scans | θmax = 27.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −4→6 |
Tmin = 0.225, Tmax = 0.557 | k = −9→9 |
1956 measured reflections | l = −10→9 |
Refinement top
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 0.93 | w = 1/[σ2(Fo2) + (0.0542P)2] where P = (Fo2 + 2Fc2)/3 |
1346 reflections | (Δ/σ)max < 0.001 |
53 parameters | Δρmax = 0.75 e Å−3 |
0 restraints | Δρmin = −0.84 e Å−3 |
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. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
N1 | 0.4626 (13) | 0.6366 (9) | 0.1389 (9) | 0.070 (3) | 0.68 (10) |
C1 | 0.4626 (13) | 0.6366 (9) | 0.1389 (9) | 0.070 (3) | 0.32 (10) |
C2 | 0.3525 (17) | 0.6049 (12) | −0.0182 (11) | 0.080 (2) | |
H2 | 0.2498 | 0.6761 | −0.0331 | 0.096* | |
C3 | 0.6100 (17) | 0.5304 (13) | 0.1554 (10) | 0.079 (2) | |
H3 | 0.6878 | 0.5497 | 0.2622 | 0.094* | |
C4 | 0.4213 (19) | 0.7812 (15) | 0.2901 (12) | 0.098 (3) | |
H4A | 0.5213 | 0.7873 | 0.3888 | 0.148* | |
H4B | 0.2406 | 0.7447 | 0.3013 | 0.148* | |
H4C | 0.4752 | 0.9048 | 0.2776 | 0.148* | |
I1 | 0.05217 (13) | 0.26565 (8) | 0.34224 (7) | 0.0949 (3) | |
I2 | 0.0000 | 0.0000 | 0.0000 | 0.0669 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
N1 | 0.070 (5) | 0.073 (5) | 0.068 (5) | 0.025 (4) | 0.017 (3) | 0.023 (4) |
C1 | 0.070 (5) | 0.073 (5) | 0.068 (5) | 0.025 (4) | 0.017 (3) | 0.023 (4) |
C2 | 0.091 (6) | 0.090 (6) | 0.073 (6) | 0.050 (5) | 0.010 (5) | 0.027 (5) |
C3 | 0.079 (6) | 0.097 (6) | 0.060 (5) | 0.036 (5) | 0.001 (4) | 0.022 (4) |
C4 | 0.117 (8) | 0.092 (6) | 0.081 (6) | 0.045 (5) | 0.030 (5) | 0.012 (5) |
I1 | 0.1301 (6) | 0.0918 (5) | 0.0515 (4) | 0.0402 (4) | 0.0162 (3) | 0.0066 (3) |
I2 | 0.0878 (6) | 0.0609 (4) | 0.0579 (4) | 0.0338 (4) | 0.0159 (3) | 0.0192 (3) |
Geometric parameters (Å, º) top
N1—C3 | 1.349 (10) | C3—H3 | 0.9300 |
N1—C2 | 1.351 (10) | C4—H4A | 0.9600 |
N1—C4 | 1.488 (11) | C4—H4B | 0.9600 |
C2—C3i | 1.368 (12) | C4—H4C | 0.9600 |
C2—H2 | 0.9300 | I1—I2 | 2.916 (1) |
C3—C2i | 1.368 (12) | I2—I1ii | 2.9159 (11) |
| | | |
C3—N1—C2 | 117.8 (7) | C2i—C3—H3 | 119.3 |
C3—N1—C4 | 120.5 (8) | N1—C4—H4A | 109.5 |
C2—N1—C4 | 121.7 (7) | N1—C4—H4B | 109.5 |
N1—C2—C3i | 120.9 (7) | H4A—C4—H4B | 109.5 |
N1—C2—H2 | 119.6 | N1—C4—H4C | 109.5 |
C3i—C2—H2 | 119.6 | H4A—C4—H4C | 109.5 |
N1—C3—C2i | 121.4 (8) | H4B—C4—H4C | 109.5 |
N1—C3—H3 | 119.3 | I1ii—I2—I1 | 180.00 (4) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y, −z. |
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