Download citation
Download citation
link to html
Crystals of the one-dimensional organic–inorganic lead iodide-based compound N-isopropyl­idenepropanaminium triiodo­plumbate(II), (C6H14N)[PbI3], were prepared by slow evaporation at room temperature. In the inorganic sublattice, the PbI6 octa­hedra form infinite one-dimensional chains sharing triangular faces. The inorganic PbI3 chain and the organic cations are connected through N—H...I hydrogen-bonding inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680605392X/dn2098sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680605392X/dn2098Isup2.hkl
Contains datablock I

CCDC reference: 636241

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.027 Å
  • R factor = 0.055
  • wR factor = 0.152
  • Data-to-parameter ratio = 31.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 28
Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C4 PLAT420_ALERT_2_C D-H Without Acceptor N - H1 ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H1 .. I2 .. 3.09 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H1 .. I3 .. 3.25 Ang.
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 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 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 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

Computing details top

Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

N-isopropylidenepropanaminium triiodoplumbate top
Crystal data top
(C6H14N)[PbI3]F(000) = 1192
Mr = 688.07Dx = 3.094 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 11.533 (4) Åθ = 11–20°
b = 16.291 (5) ŵ = 17.65 mm1
c = 8.251 (3) ÅT = 293 K
β = 107.66 (3)°Parallelipiped, yellow
V = 1477.2 (9) Å30.24 × 0.16 × 0.12 mm
Z = 4
Data collection top
Enraf–Nonius CAD-4
diffractometer
2058 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.081
Graphite monochromatorθmax = 27.0°, θmin = 2.2°
ω/2θ scansh = 014
Absorption correction: ψ scan
(North et al., 1968)
k = 200
Tmin = 0.045, Tmax = 0.126l = 1010
5585 measured reflections2 standard reflections every 120 min
3207 independent reflections intensity decay: 2%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.152H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0773P)2]
where P = (Fo2 + 2Fc2)/3
3207 reflections(Δ/σ)max < 0.001
103 parametersΔρmax = 3.92 e Å3
0 restraintsΔρmin = 2.37 e Å3
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
Pb0.19037 (5)0.75154 (3)0.56129 (6)0.03966 (19)
I10.00854 (9)0.67843 (8)0.71550 (12)0.0521 (3)
I20.39061 (9)0.66833 (8)0.88216 (12)0.0533 (3)
I30.19895 (9)0.59649 (7)0.34799 (11)0.0492 (3)
C10.2476 (18)0.4058 (15)1.061 (2)0.084 (7)
H1A0.23800.35021.02050.126*
H1B0.23220.40871.16870.126*
H1C0.32920.42381.07380.126*
C20.1585 (17)0.4606 (12)0.934 (2)0.066 (5)
H2A0.18270.51740.95960.079*
H2B0.07860.45400.94840.079*
C30.1491 (14)0.4434 (15)0.749 (2)0.070 (6)
H3A0.12030.38770.72120.084*
H3B0.08960.48030.67670.084*
C40.3383 (15)0.4013 (13)0.6818 (18)0.060 (5)
C50.3162 (16)0.3112 (15)0.681 (2)0.081 (7)
H5A0.25420.30010.73340.122*
H5B0.39000.28380.74250.122*
H5C0.29010.29170.56550.122*
C60.4485 (19)0.4319 (17)0.650 (3)0.096 (8)
H6A0.44510.49070.64200.144*
H6B0.45470.40920.54580.144*
H6C0.51840.41590.74230.144*
N0.2647 (14)0.4535 (10)0.7133 (17)0.065 (4)
H10.28780.50370.71340.078*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb0.0404 (3)0.0456 (4)0.0332 (3)0.0002 (3)0.0115 (2)0.0011 (2)
I10.0402 (6)0.0678 (8)0.0475 (5)0.0125 (5)0.0120 (4)0.0054 (5)
I20.0368 (6)0.0647 (8)0.0538 (5)0.0090 (5)0.0069 (4)0.0033 (5)
I30.0628 (7)0.0412 (6)0.0449 (5)0.0028 (5)0.0182 (4)0.0013 (4)
C10.073 (13)0.11 (2)0.079 (12)0.040 (14)0.045 (10)0.002 (12)
C20.060 (12)0.057 (13)0.090 (12)0.004 (9)0.037 (9)0.015 (9)
C30.023 (8)0.112 (17)0.077 (10)0.004 (10)0.019 (7)0.022 (11)
C40.054 (10)0.082 (15)0.048 (8)0.026 (10)0.023 (7)0.012 (8)
C50.049 (12)0.077 (18)0.102 (15)0.021 (11)0.001 (10)0.018 (11)
C60.077 (15)0.12 (2)0.115 (16)0.003 (14)0.057 (13)0.038 (15)
N0.070 (10)0.057 (11)0.068 (9)0.005 (8)0.021 (7)0.016 (7)
Geometric parameters (Å, º) top
Pb—I33.0974 (15)C3—N1.46 (2)
Pb—I13.1735 (14)C3—H3A0.9700
Pb—I23.2359 (17)C3—H3B0.9700
Pb—I1i3.2761 (17)C4—N1.28 (2)
Pb—I2i3.3605 (15)C4—C61.46 (2)
Pb—I3ii3.4048 (17)C4—C51.49 (3)
C1—C21.52 (3)C5—H5A0.9600
C1—H1A0.9600C5—H5B0.9600
C1—H1B0.9600C5—H5C0.9600
C1—H1C0.9600C6—H6A0.9600
C2—C31.52 (2)C6—H6B0.9600
C2—H2A0.9700C6—H6C0.9600
C2—H2B0.9700N—H10.8600
I3—Pb—I194.20 (4)C1—C2—H2B108.7
I3—Pb—I289.16 (4)C3—C2—H2B108.7
I1—Pb—I286.45 (4)H2A—C2—H2B107.6
I3—Pb—I1i85.63 (4)N—C3—C2113.0 (13)
I1—Pb—I1i94.56 (5)N—C3—H3A109.0
I2—Pb—I1i174.75 (3)C2—C3—H3A109.0
I3—Pb—I2i85.54 (4)N—C3—H3B109.0
I1—Pb—I2i177.37 (3)C2—C3—H3B109.0
I2—Pb—I2i96.17 (4)H3A—C3—H3B107.8
I1i—Pb—I2i82.81 (4)N—C4—C6118 (2)
I3—Pb—I3ii171.33 (3)N—C4—C5122.1 (18)
I1—Pb—I3ii82.33 (4)C6—C4—C5119.5 (18)
I2—Pb—I3ii82.71 (4)C4—C5—H5A109.5
I1i—Pb—I3ii102.53 (4)C4—C5—H5B109.5
I2i—Pb—I3ii98.28 (4)H5A—C5—H5B109.5
Pb—I1—Pbii79.52 (4)C4—C5—H5C109.5
Pb—I2—Pbii77.41 (4)H5A—C5—H5C109.5
Pb—I3—Pbi78.61 (4)H5B—C5—H5C109.5
C2—C1—H1A109.5C4—C6—H6A109.5
C2—C1—H1B109.5C4—C6—H6B109.5
H1A—C1—H1B109.5H6A—C6—H6B109.5
C2—C1—H1C109.5C4—C6—H6C109.5
H1A—C1—H1C109.5H6A—C6—H6C109.5
H1B—C1—H1C109.5H6B—C6—H6C109.5
C1—C2—C3114.2 (15)C4—N—C3132 (2)
C1—C2—H2A108.7C4—N—H1114.0
C3—C2—H2A108.7C3—N—H1114.0
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N—H1···I20.863.093.882 (17)155
N—H1···I30.863.253.702 (14)116
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds