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The crystal structure of the title compound, C3H10N+·I, originally determined by Sheldrick & Sheldrick [Acta Cryst. (1970), B26, 1334–1338], has been redetermined at 93 K. Both ions lie on a mirror plane. They form N—H...I hydrogen-bonded units in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806030261/bt2152sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806030261/bt2152Isup2.hkl
Contains datablock I

CCDC reference: 620677

Key indicators

  • Single-crystal X-ray study
  • T = 93 K
  • Mean [sigma](N-C) = 0.002 Å
  • R factor = 0.010
  • wR factor = 0.024
  • Data-to-parameter ratio = 14.4

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.90
Author Response: ... Data collection was not a complete sphere because of instrument limitations; more than adequate redundant data was collected as indicated by final R factors.

Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 27.94 From the CIF: _diffrn_reflns_theta_full 27.94 From the CIF: _reflns_number_total 735 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 813 Completeness (_total/calc) 90.41% PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 5
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Siemens, 2001); cell refinement: SMART; data reduction: SAINT (Siemens, 2001) and SADABS (Sheldrick, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997).

trimethylammonium iodide top
Crystal data top
C3H10N+·IF(000) = 176
Mr = 187.02Dx = 1.969 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 1695 reflections
a = 5.5309 (7) Åθ = 2.5–28.0°
b = 8.2737 (10) ŵ = 4.94 mm1
c = 7.1000 (9) ÅT = 93 K
β = 103.801 (1)°Block, colourless
V = 315.52 (7) Å30.37 × 0.18 × 0.16 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
735 independent reflections
Radiation source: fine-focus sealed tube730 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.011
Detector resolution: 8.192 pixels mm-1θmax = 27.9°, θmin = 3.0°
φ and ω scansh = 67
Absorption correction: multi-scan
(Blessing, 1995)
k = 1010
Tmin = 0.304, Tmax = 0.454l = 59
1741 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.010All H-atom parameters refined
wR(F2) = 0.024 w = 1/[σ2(Fo2) + (0.0077P)2 + 0.1167P]
where P = (Fo2 + 2Fc2)/3
S = 1.23(Δ/σ)max = 0.001
735 reflectionsΔρmax = 0.34 e Å3
51 parametersΔρmin = 0.25 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.045 (2)
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
xyzUiso*/Ueq
I10.03818 (2)0.25000.203342 (18)0.01281 (8)
N10.5629 (3)0.25000.7777 (3)0.0133 (3)
C10.7161 (4)0.25000.6300 (3)0.0183 (4)
C20.4065 (3)0.10057 (18)0.7625 (2)0.0163 (3)
H10.607 (5)0.25000.507 (4)0.015 (6)*
H20.815 (4)0.155 (2)0.647 (3)0.022 (5)*
H30.662 (6)0.25000.882 (5)0.022 (7)*
H40.298 (3)0.100 (2)0.639 (3)0.015 (4)*
H50.310 (3)0.105 (2)0.863 (3)0.016 (5)*
H60.521 (4)0.006 (3)0.779 (3)0.021 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.01116 (10)0.01505 (10)0.01131 (10)0.0000.00088 (5)0.000
N10.0097 (8)0.0177 (9)0.0112 (9)0.0000.0002 (7)0.000
C10.0143 (10)0.0242 (11)0.0180 (11)0.0000.0069 (9)0.000
C20.0158 (7)0.0148 (7)0.0177 (7)0.0007 (6)0.0027 (6)0.0013 (6)
Geometric parameters (Å, º) top
N1—C11.498 (3)C1—H20.95 (2)
N1—C21.4977 (18)C2—H40.94 (2)
N1—C2i1.4977 (18)C2—H50.99 (2)
N1—H30.81 (3)C2—H61.00 (2)
C1—H10.94 (3)
C1—N1—C2111.26 (11)H1—C1—H2110.2 (15)
C1—N1—C2i111.26 (11)N1—C2—H4107.6 (11)
C2—N1—C2i111.27 (17)N1—C2—H5108.5 (11)
C1—N1—H3105 (2)H4—C2—H5110.0 (16)
C2—N1—H3108.7 (11)N1—C2—H6107.6 (12)
C2i—N1—H3108.7 (11)H4—C2—H6110.5 (16)
N1—C1—H1107.9 (17)H5—C2—H6112.3 (16)
N1—C1—H2108.4 (13)
Symmetry code: (i) x, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H3···I1ii0.81 (3)2.70 (3)3.500 (2)173 (3)
Symmetry code: (ii) x+1, y, z+1.
 

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