Three inorganic-organic layered perovskite-type hybrids of the general formula [(CnH2n + 1NH3)2PbI4], n = 4, 5 and 6, display a number of reversible first-order phase transitions in the temperature range from 256 to 393 K. [(C4H9NH3)2PbI4] has a single phase transition, [(C5H11NH3)2PbI4] has two phase transitions and [(C6H13NH3)2PbI4] has three phase transitions. In all three cases, the lowest-temperature phase transition is thermochromic and the crystals change colour from yellow in their lowest-temperature phase to orange in their higher-temperature phase for [(C4H9NH3)2PbI4] and [(C6H13NH3)2PbI4], and from orange to red for [(C5H11NH3)2PbI4]. The structural details associated with this phase transition have been investigated via single-crystal X-ray diffraction, SC-XRD, for all three compounds.
Supporting information
CCDC references: 665689; 665690; 665691; 665692; 665693; 665694; 665695
For all compounds, data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus and XPREP (Bruker 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003).
(1a) bis(butylammonium)tetraiodoplumbate(II)
top
Crystal data top
2(C4H12N)·I4Pb | F(000) = 1520 |
Mr = 863.08 | Dx = 2.886 Mg m−3 Dm = 0 Mg m−3 Dm measured by not measured |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 3361 reflections |
a = 8.4280 (19) Å | θ = 3.1–28.2° |
b = 8.986 (2) Å | µ = 14.69 mm−1 |
c = 26.233 (6) Å | T = 223 K |
V = 1986.7 (8) Å3 | Cube, yellow |
Z = 4 | 0.14 × 0.13 × 0.08 mm |
Data collection top
Bruker APEX II CCD area detector diffractometer | 1745 independent reflections |
Radiation source: fine-focus sealed tube | 1500 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.083 |
ω scans | θmax = 25°, θmin = 2.9° |
Absorption correction: integration Bruker XPREP (Bruker, 2004) | h = −10→9 |
Tmin = 0.165, Tmax = 0.339 | k = −10→10 |
7581 measured reflections | l = −31→29 |
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)] = 0.101 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.27 | H-atom parameters constrained |
S = 1.38 | w = 1/[σ2(Fo2) + (0.P)2 + 573.3984P] where P = (Fo2 + 2Fc2)/3 |
1745 reflections | (Δ/σ)max < 0.001 |
70 parameters | Δρmax = 3.92 e Å−3 |
31 restraints | Δρmin = −5.68 e Å−3 |
Special details top
Experimental. Numerical integration absorption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 2004) |
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 | |
C1 | 0.925 (5) | 0.440 (4) | 0.8573 (17) | 0.033 (7) | |
H1D | 0.8115 | 0.4325 | 0.8657 | 0.04* | |
H1E | 0.9508 | 0.3574 | 0.8342 | 0.04* | |
C2 | 0.957 (5) | 0.587 (5) | 0.8307 (17) | 0.038 (7) | |
H2A | 1.0671 | 0.5885 | 0.8188 | 0.045* | |
H2B | 0.9448 | 0.6682 | 0.8555 | 0.045* | |
C3 | 0.846 (6) | 0.618 (5) | 0.7849 (17) | 0.042 (8) | |
H3A | 0.8527 | 0.5345 | 0.7609 | 0.051* | |
H3B | 0.7363 | 0.6246 | 0.7969 | 0.051* | |
C4 | 0.889 (6) | 0.756 (5) | 0.7586 (19) | 0.046 (10) | |
H4A | 0.817 | 0.772 | 0.7303 | 0.069* | |
H4B | 0.9968 | 0.7484 | 0.7459 | 0.069* | |
H4C | 0.8815 | 0.8387 | 0.7822 | 0.069* | |
N1 | 1.016 (4) | 0.427 (3) | 0.9025 (13) | 0.030 (7) | |
H1A | 0.9957 | 0.3391 | 0.9175 | 0.045* | |
H1B | 0.9905 | 0.5015 | 0.9239 | 0.045* | |
H1C | 1.1198 | 0.4326 | 0.8947 | 0.045* | |
I1 | 1.0779 (3) | 1.0298 (3) | 0.88221 (10) | 0.0314 (7) | |
I2 | 0.6987 (3) | 1.2042 (3) | 0.97709 (11) | 0.0311 (7) | |
Pb1 | 1 | 1 | 1 | 0.0237 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.027 (15) | 0.023 (13) | 0.050 (16) | 0.015 (13) | 0.004 (12) | −0.003 (11) |
C2 | 0.031 (15) | 0.034 (14) | 0.049 (15) | 0.012 (13) | 0.002 (13) | 0.005 (11) |
C3 | 0.039 (17) | 0.040 (16) | 0.048 (17) | 0.016 (15) | 0.000 (14) | 0.002 (13) |
C4 | 0.05 (2) | 0.039 (18) | 0.05 (2) | 0.019 (18) | −0.009 (19) | 0.006 (15) |
N1 | 0.036 (18) | 0.009 (13) | 0.046 (16) | 0.000 (13) | 0.001 (13) | −0.004 (11) |
I1 | 0.0287 (14) | 0.0282 (13) | 0.0374 (15) | 0.0022 (11) | 0.0016 (12) | 0.0010 (11) |
I2 | 0.0217 (12) | 0.0268 (13) | 0.0448 (15) | 0.0116 (10) | 0.0014 (11) | 0.0009 (12) |
Pb1 | 0.0196 (10) | 0.0180 (9) | 0.0334 (11) | 0.0001 (8) | −0.0006 (9) | 0.0019 (9) |
Geometric parameters (Å, º) top
C1—N1 | 1.42 (5) | C4—H4C | 0.97 |
C1—C2 | 1.53 (6) | N1—H1A | 0.9 |
C1—H1D | 0.98 | N1—H1B | 0.9 |
C1—H1E | 0.98 | N1—H1C | 0.9 |
C2—C3 | 1.55 (6) | I1—Pb1 | 3.170 (3) |
C2—H2A | 0.98 | I2—Pb1 | 3.190 (2) |
C2—H2B | 0.98 | I2—Pb1i | 3.199 (2) |
C3—C4 | 1.46 (6) | Pb1—I1ii | 3.170 (3) |
C3—H3A | 0.98 | Pb1—I2ii | 3.190 (2) |
C3—H3B | 0.98 | Pb1—I2iii | 3.199 (2) |
C4—H4A | 0.97 | Pb1—I2iv | 3.199 (2) |
C4—H4B | 0.97 | | |
| | | |
N1—C1—C2 | 111 (4) | H4B—C4—H4C | 109.5 |
N1—C1—H1D | 109.5 | C1—N1—H1A | 109.5 |
C2—C1—H1D | 109.5 | C1—N1—H1B | 109.5 |
N1—C1—H1E | 109.5 | H1A—N1—H1B | 109.5 |
C2—C1—H1E | 109.5 | C1—N1—H1C | 109.5 |
H1D—C1—H1E | 108.1 | H1A—N1—H1C | 109.5 |
C1—C2—C3 | 114 (4) | H1B—N1—H1C | 109.5 |
C1—C2—H2A | 108.8 | Pb1—I2—Pb1i | 149.24 (10) |
C3—C2—H2A | 108.8 | I1ii—Pb1—I1 | 180.0000 (10) |
C1—C2—H2B | 108.8 | I1ii—Pb1—I2ii | 86.15 (7) |
C3—C2—H2B | 108.8 | I1—Pb1—I2ii | 93.85 (7) |
H2A—C2—H2B | 107.7 | I1ii—Pb1—I2 | 93.85 (7) |
C4—C3—C2 | 111 (4) | I1—Pb1—I2 | 86.15 (7) |
C4—C3—H3A | 109.3 | I2ii—Pb1—I2 | 180.0000 (10) |
C2—C3—H3A | 109.3 | I1ii—Pb1—I2iii | 90.26 (7) |
C4—C3—H3B | 109.3 | I1—Pb1—I2iii | 89.74 (7) |
C2—C3—H3B | 109.3 | I2ii—Pb1—I2iii | 88.52 (3) |
H3A—C3—H3B | 108 | I2—Pb1—I2iii | 91.48 (3) |
C3—C4—H4A | 109.5 | I1ii—Pb1—I2iv | 89.74 (7) |
C3—C4—H4B | 109.5 | I1—Pb1—I2iv | 90.26 (7) |
H4A—C4—H4B | 109.5 | I2ii—Pb1—I2iv | 91.48 (3) |
C3—C4—H4C | 109.5 | I2—Pb1—I2iv | 88.52 (3) |
H4A—C4—H4C | 109.5 | I2iii—Pb1—I2iv | 180 |
| | | |
N1—C1—C2—C3 | −173 (3) | Pb1i—I2—Pb1—I1 | −123.18 (19) |
C1—C2—C3—C4 | −176 (4) | Pb1i—I2—Pb1—I2iii | 147.18 (15) |
Pb1i—I2—Pb1—I1ii | 56.82 (19) | Pb1i—I2—Pb1—I2iv | −32.82 (15) |
Symmetry codes: (i) x−1/2, −y+5/2, −z+2; (ii) −x+2, −y+2, −z+2; (iii) −x+3/2, y−1/2, z; (iv) x+1/2, −y+5/2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I1v | 0.9 | 3.01 | 3.65 (3) | 129 |
N1—H1B···I2iii | 0.9 | 2.79 | 3.65 (3) | 159 |
N1—H1C···I1vi | 0.9 | 2.71 | 3.58 (3) | 163 |
Symmetry codes: (iii) −x+3/2, y−1/2, z; (v) x, y−1, z; (vi) −x+5/2, y−1/2, z. |
(1b) bis(butylammonium)tetraiodoplumbate(II)
top
Crystal data top
2(C4H12N)·I4Pb | F(000) = 1520 |
Mr = 863.08 | Dx = 2.692 Mg m−3 Dm = 0 Mg m−3 Dm measured by not measured |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 4303 reflections |
a = 8.8764 (1) Å | θ = 2.7–28.0° |
b = 8.6925 (1) Å | µ = 13.71 mm−1 |
c = 27.6014 (5) Å | T = 293 K |
V = 2129.67 (5) Å3 | Cube, orange |
Z = 4 | 0.15 × 0.14 × 0.08 mm |
Data collection top
Bruker APEX II CCD area detector diffractometer | 1981 independent reflections |
Radiation source: fine-focus sealed tube | 1541 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.079 |
ω scans | θmax = 25.5°, θmin = 2.7° |
Absorption correction: integration Bruker XPREP (Bruker, 2004) | h = −10→10 |
Tmin = 0.160, Tmax = 0.359 | k = −10→10 |
15579 measured reflections | l = −33→32 |
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)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0196P)2 + 10.8314P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max = 0.001 |
1981 reflections | Δρmax = 0.82 e Å−3 |
71 parameters | Δρmin = −1.15 e Å−3 |
36 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00341 (14) |
Special details top
Experimental. Numerical integration absorption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 2004) |
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 | |
C1 | 0.9692 (19) | 0.4748 (18) | 0.8819 (5) | 0.150 (5) | |
H1D | 0.8679 | 0.5025 | 0.8918 | 0.18* | |
H1E | 0.9871 | 0.3691 | 0.8916 | 0.18* | |
C2 | 0.9822 (18) | 0.4879 (19) | 0.8282 (5) | 0.176 (6) | |
H2A | 1.0827 | 0.4579 | 0.818 | 0.212* | |
H2B | 0.9659 | 0.5938 | 0.8184 | 0.212* | |
C3 | 0.866 (2) | 0.384 (2) | 0.8039 (6) | 0.210 (7) | |
H3A | 0.8749 | 0.2808 | 0.8167 | 0.252* | |
H3B | 0.7655 | 0.4215 | 0.8114 | 0.252* | |
C4 | 0.886 (3) | 0.380 (3) | 0.7509 (6) | 0.283 (11) | |
H4A | 0.8104 | 0.3143 | 0.7368 | 0.424* | |
H4B | 0.9839 | 0.341 | 0.7433 | 0.424* | |
H4C | 0.8751 | 0.4821 | 0.738 | 0.424* | |
N1 | 1.0761 (10) | 0.5741 (11) | 0.9059 (4) | 0.094 (3) | |
H1A | 1.0594 | 0.5726 | 0.9377 | 0.141* | |
H1B | 1.0657 | 0.6697 | 0.8949 | 0.141* | |
H1C | 1.1692 | 0.5412 | 0.8999 | 0.141* | |
I1 | 1.03349 (8) | 0.98557 (8) | 0.88455 (3) | 0.0782 (3) | |
I2 | 0.69648 (7) | 1.19465 (7) | 0.99571 (3) | 0.0711 (3) | |
Pb1 | 1 | 1 | 1 | 0.04801 (18) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.139 (11) | 0.157 (13) | 0.155 (9) | −0.035 (9) | −0.010 (10) | −0.033 (10) |
C2 | 0.174 (13) | 0.206 (14) | 0.149 (8) | −0.008 (11) | −0.032 (10) | −0.044 (11) |
C3 | 0.199 (15) | 0.258 (17) | 0.172 (11) | −0.028 (13) | −0.041 (12) | −0.062 (13) |
C4 | 0.29 (3) | 0.39 (3) | 0.166 (12) | −0.04 (3) | −0.051 (17) | −0.08 (2) |
N1 | 0.074 (6) | 0.095 (7) | 0.113 (7) | 0.010 (5) | −0.005 (5) | −0.004 (5) |
I1 | 0.0784 (5) | 0.0804 (5) | 0.0756 (5) | 0.0008 (4) | −0.0086 (3) | 0.0035 (4) |
I2 | 0.0482 (3) | 0.0474 (3) | 0.1176 (6) | 0.0195 (3) | −0.0124 (3) | −0.0075 (4) |
Pb1 | 0.0338 (2) | 0.0347 (2) | 0.0755 (3) | 0.00014 (16) | −0.00003 (19) | 0.0008 (2) |
Geometric parameters (Å, º) top
C1—N1 | 1.443 (16) | C4—H4C | 0.96 |
C1—C2 | 1.493 (9) | N1—H1A | 0.89 |
C1—H1D | 0.97 | N1—H1B | 0.89 |
C1—H1E | 0.97 | N1—H1C | 0.89 |
C2—C3 | 1.526 (9) | I1—Pb1 | 3.2029 (7) |
C2—H2A | 0.97 | I2—Pb1i | 3.1781 (5) |
C2—H2B | 0.97 | I2—Pb1 | 3.1836 (5) |
C3—C4 | 1.475 (10) | Pb1—I2ii | 3.1781 (5) |
C3—H3A | 0.97 | Pb1—I2iii | 3.1781 (5) |
C3—H3B | 0.97 | Pb1—I2iv | 3.1836 (5) |
C4—H4A | 0.96 | Pb1—I1iv | 3.2029 (7) |
C4—H4B | 0.96 | | |
| | | |
N1—C1—C2 | 111.1 (12) | H4B—C4—H4C | 109.5 |
N1—C1—H1D | 109.4 | C1—N1—H1A | 109.5 |
C2—C1—H1D | 109.4 | C1—N1—H1B | 109.5 |
N1—C1—H1E | 109.4 | H1A—N1—H1B | 109.5 |
C2—C1—H1E | 109.4 | C1—N1—H1C | 109.5 |
H1D—C1—H1E | 108 | H1A—N1—H1C | 109.5 |
C1—C2—C3 | 109.8 (11) | H1B—N1—H1C | 109.5 |
C1—C2—H2A | 109.7 | Pb1i—I2—Pb1 | 155.08 (2) |
C3—C2—H2A | 109.7 | I2ii—Pb1—I2iii | 180 |
C1—C2—H2B | 109.7 | I2ii—Pb1—I2 | 91.256 (4) |
C3—C2—H2B | 109.7 | I2iii—Pb1—I2 | 88.744 (4) |
H2A—C2—H2B | 108.2 | I2ii—Pb1—I2iv | 88.744 (4) |
C4—C3—C2 | 111.7 (12) | I2iii—Pb1—I2iv | 91.256 (4) |
C4—C3—H3A | 109.3 | I2—Pb1—I2iv | 180 |
C2—C3—H3A | 109.3 | I2ii—Pb1—I1 | 91.077 (18) |
C4—C3—H3B | 109.3 | I2iii—Pb1—I1 | 88.922 (18) |
C2—C3—H3B | 109.3 | I2—Pb1—I1 | 93.576 (19) |
H3A—C3—H3B | 107.9 | I2iv—Pb1—I1 | 86.424 (19) |
C3—C4—H4A | 109.5 | I2ii—Pb1—I1iv | 88.923 (18) |
C3—C4—H4B | 109.5 | I2iii—Pb1—I1iv | 91.078 (18) |
H4A—C4—H4B | 109.5 | I2—Pb1—I1iv | 86.424 (19) |
C3—C4—H4C | 109.5 | I2iv—Pb1—I1iv | 93.576 (19) |
H4A—C4—H4C | 109.5 | I1—Pb1—I1iv | 180 |
| | | |
N1—C1—C2—C3 | −178.9 (15) | Pb1i—I2—Pb1—I2iii | 172.39 (5) |
C1—C2—C3—C4 | −173.6 (19) | Pb1i—I2—Pb1—I1 | −98.77 (6) |
Pb1i—I2—Pb1—I2ii | −7.61 (5) | Pb1i—I2—Pb1—I1iv | 81.23 (6) |
Symmetry codes: (i) x−1/2, −y+5/2, −z+2; (ii) x+1/2, −y+5/2, −z+2; (iii) −x+3/2, y−1/2, z; (iv) −x+2, −y+2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I2iii | 0.89 | 2.97 | 3.619 (9) | 131 |
N1—H1B···I1 | 0.89 | 2.77 | 3.645 (9) | 166 |
N1—H1C···I1v | 0.89 | 2.72 | 3.598 (9) | 171 |
Symmetry codes: (iii) −x+3/2, y−1/2, z; (v) −x+5/2, y−1/2, z. |
(2a) bis(pentylammonium)tetraiodoplumbate(II)
top
Crystal data top
2(C5H14N)·I4Pb | F(000) = 792 |
Mr = 891.13 | Dx = 2.671 Mg m−3 |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yab | Cell parameters from 843 reflections |
a = 8.4716 (18) Å | θ = 3.4–28.3° |
b = 9.007 (2) Å | µ = 13.18 mm−1 |
c = 14.784 (3) Å | T = 173 K |
β = 100.881 (4)° | Rectangular, yellow |
V = 1107.8 (4) Å3 | 0.58 × 0.32 × 0.11 mm |
Z = 2 | |
Data collection top
Bruker APEX II CCD area detector diffractometer | 2649 independent reflections |
Radiation source: fine-focus sealed tube | 2334 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.080 |
ω scans | θmax = 28°, θmin = 2.7° |
Absorption correction: integration Bruker XPREP (Bruker, 2004) | h = −11→11 |
Tmin = 0.035, Tmax = 0.241 | k = −11→11 |
7043 measured reflections | l = −13→19 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.15 | w = 1/[σ2(Fo2) + (0.0375P)2 + 8.7673P] where P = (Fo2 + 2Fc2)/3 |
2649 reflections | (Δ/σ)max = 0.001 |
79 parameters | Δρmax = 1.50 e Å−3 |
0 restraints | Δρmin = −2.67 e Å−3 |
Special details top
Experimental. Numerical integration absorption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 2004) |
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 | |
C1 | 0.9329 (13) | 0.5152 (11) | 0.7377 (8) | 0.037 (2) | |
H1D | 1.0511 | 0.5252 | 0.7453 | 0.045* | |
H1E | 0.8834 | 0.5938 | 0.6947 | 0.045* | |
C2 | 0.8840 (14) | 0.3669 (12) | 0.6962 (7) | 0.041 (2) | |
H2A | 0.7683 | 0.3504 | 0.6957 | 0.05* | |
H2B | 0.9454 | 0.2879 | 0.734 | 0.05* | |
C3 | 0.9160 (17) | 0.3578 (13) | 0.5954 (9) | 0.053 (3) | |
H3A | 0.8443 | 0.4293 | 0.5567 | 0.063* | |
H3B | 1.0282 | 0.3889 | 0.5957 | 0.063* | |
C4 | 0.8908 (18) | 0.2087 (14) | 0.5526 (8) | 0.052 (3) | |
H4A | 0.7806 | 0.1744 | 0.555 | 0.063* | |
H4B | 0.9674 | 0.1378 | 0.5885 | 0.063* | |
C5 | 0.9136 (16) | 0.2087 (17) | 0.4539 (8) | 0.057 (3) | |
H5A | 0.8956 | 0.1084 | 0.4284 | 0.086* | |
H5B | 1.0233 | 0.2404 | 0.4513 | 0.086* | |
H5C | 0.8366 | 0.2773 | 0.4178 | 0.086* | |
N1 | 0.8865 (11) | 0.5381 (9) | 0.8266 (6) | 0.0353 (17) | |
H1A | 0.9175 | 0.6304 | 0.848 | 0.053* | |
H1B | 0.935 | 0.4687 | 0.8673 | 0.053* | |
H1C | 0.7779 | 0.5296 | 0.8202 | 0.053* | |
I1 | 0.95279 (8) | 0.92483 (6) | 0.78682 (4) | 0.03160 (16) | |
I2 | 0.68969 (6) | 1.20798 (6) | 0.95764 (4) | 0.02885 (15) | |
Pb1 | 1 | 1 | 1 | 0.01954 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.040 (5) | 0.032 (5) | 0.042 (5) | 0.000 (4) | 0.014 (5) | −0.001 (4) |
C2 | 0.043 (5) | 0.034 (5) | 0.046 (6) | 0.007 (4) | 0.006 (5) | −0.012 (5) |
C3 | 0.060 (7) | 0.040 (6) | 0.061 (7) | 0.001 (5) | 0.020 (6) | −0.001 (6) |
C4 | 0.068 (8) | 0.048 (6) | 0.040 (6) | −0.010 (6) | 0.009 (6) | −0.007 (5) |
C5 | 0.056 (7) | 0.077 (9) | 0.039 (6) | −0.003 (7) | 0.011 (5) | −0.018 (6) |
N1 | 0.043 (5) | 0.029 (4) | 0.032 (4) | 0.005 (3) | 0.003 (4) | −0.006 (3) |
I1 | 0.0394 (3) | 0.0272 (3) | 0.0276 (3) | −0.0040 (2) | 0.0048 (2) | −0.0025 (2) |
I2 | 0.0226 (3) | 0.0234 (3) | 0.0406 (3) | 0.00983 (19) | 0.0060 (2) | 0.0005 (2) |
Pb1 | 0.01671 (19) | 0.01495 (18) | 0.0271 (2) | 0.00023 (13) | 0.00451 (15) | −0.00109 (15) |
Geometric parameters (Å, º) top
C1—N1 | 1.457 (13) | C5—H5A | 0.98 |
C1—C2 | 1.496 (14) | C5—H5B | 0.98 |
C1—H1D | 0.99 | C5—H5C | 0.98 |
C1—H1E | 0.99 | N1—H1A | 0.91 |
C2—C3 | 1.565 (16) | N1—H1B | 0.91 |
C2—H2A | 0.99 | N1—H1C | 0.91 |
C2—H2B | 0.99 | I1—Pb1 | 3.1743 (9) |
C3—C4 | 1.483 (16) | I2—Pb1 | 3.1923 (7) |
C3—H3A | 0.99 | I2—Pb1i | 3.2052 (7) |
C3—H3B | 0.99 | Pb1—I1ii | 3.1743 (9) |
C4—C5 | 1.508 (15) | Pb1—I2ii | 3.1923 (7) |
C4—H4A | 0.99 | Pb1—I2iii | 3.2052 (7) |
C4—H4B | 0.99 | Pb1—I2iv | 3.2052 (7) |
| | | |
N1—C1—C2 | 113.3 (9) | H5A—C5—H5B | 109.5 |
N1—C1—H1D | 108.9 | C4—C5—H5C | 109.5 |
C2—C1—H1D | 108.9 | H5A—C5—H5C | 109.5 |
N1—C1—H1E | 108.9 | H5B—C5—H5C | 109.5 |
C2—C1—H1E | 108.9 | C1—N1—H1A | 109.5 |
H1D—C1—H1E | 107.7 | C1—N1—H1B | 109.5 |
C1—C2—C3 | 110.7 (9) | H1A—N1—H1B | 109.5 |
C1—C2—H2A | 109.5 | C1—N1—H1C | 109.5 |
C3—C2—H2A | 109.5 | H1A—N1—H1C | 109.5 |
C1—C2—H2B | 109.5 | H1B—N1—H1C | 109.5 |
C3—C2—H2B | 109.5 | Pb1—I2—Pb1i | 150.22 (2) |
H2A—C2—H2B | 108.1 | I1—Pb1—I1ii | 180 |
C4—C3—C2 | 114.6 (10) | I1—Pb1—I2 | 89.177 (16) |
C4—C3—H3A | 108.6 | I1ii—Pb1—I2 | 90.823 (16) |
C2—C3—H3A | 108.6 | I1—Pb1—I2ii | 90.823 (16) |
C4—C3—H3B | 108.6 | I1ii—Pb1—I2ii | 89.177 (16) |
C2—C3—H3B | 108.6 | I2—Pb1—I2ii | 180 |
H3A—C3—H3B | 107.6 | I1—Pb1—I2iii | 87.415 (17) |
C3—C4—C5 | 112.2 (11) | I1ii—Pb1—I2iii | 92.585 (17) |
C3—C4—H4A | 109.2 | I2—Pb1—I2iii | 84.535 (17) |
C5—C4—H4A | 109.2 | I2ii—Pb1—I2iii | 95.465 (17) |
C3—C4—H4B | 109.2 | I1—Pb1—I2iv | 92.585 (17) |
C5—C4—H4B | 109.2 | I1ii—Pb1—I2iv | 87.415 (17) |
H4A—C4—H4B | 107.9 | I2—Pb1—I2iv | 95.465 (17) |
C4—C5—H5A | 109.5 | I2ii—Pb1—I2iv | 84.535 (17) |
C4—C5—H5B | 109.5 | I2iii—Pb1—I2iv | 180 |
| | | |
N1—C1—C2—C3 | 172.2 (10) | Pb1i—I2—Pb1—I1ii | 34.83 (4) |
C1—C2—C3—C4 | 172.6 (11) | Pb1i—I2—Pb1—I2iii | −57.69 (5) |
C2—C3—C4—C5 | 176.6 (11) | Pb1i—I2—Pb1—I2iv | 122.31 (5) |
Pb1i—I2—Pb1—I1 | −145.17 (4) | | |
Symmetry codes: (i) −x+3/2, y+1/2, −z+2; (ii) −x+2, −y+2, −z+2; (iii) x+1/2, −y+5/2, z; (iv) −x+3/2, y−1/2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I1 | 0.91 | 2.84 | 3.594 (9) | 142 |
N1—H1B···I2v | 0.91 | 2.81 | 3.658 (9) | 156 |
N1—H1C···I1vi | 0.91 | 2.74 | 3.625 (9) | 166 |
Symmetry codes: (v) x+1/2, −y+3/2, z; (vi) x−1/2, −y+3/2, z. |
(2b) bis(pentylammonium)tetraiodoplumbate(II)
top
Crystal data top
2(C5H14N)·I4Pb | F(000) = 792 |
Mr = 891.13 | Dx = 2.61 Mg m−3 Dm = 0 Mg m−3 Dm measured by not measured |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yab | Cell parameters from 4406 reflections |
a = 8.6716 (7) Å | θ = 2.5–30.8° |
b = 8.9297 (6) Å | µ = 12.87 mm−1 |
c = 14.8805 (13) Å | T = 293 K |
β = 100.212 (2)° | Plate, orange |
V = 1134.01 (15) Å3 | 0.5 × 0.46 × 0.14 mm |
Z = 2 | |
Data collection top
Bruker APEX II CCD area detector diffractometer | 2734 independent reflections |
Radiation source: fine-focus sealed tube | 2259 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.055 |
ω scans | θmax = 28°, θmin = 1.4° |
Absorption correction: integration Bruker XPREP (Bruker, 2004) | h = −10→11 |
Tmin = 0.020, Tmax = 0.179 | k = −7→11 |
8718 measured reflections | l = −19→19 |
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) = 0.121 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0576P)2 + 5.635P] where P = (Fo2 + 2Fc2)/3 |
2734 reflections | (Δ/σ)max = 0.001 |
79 parameters | Δρmax = 1.90 e Å−3 |
46 restraints | Δρmin = −2.07 e Å−3 |
Special details top
Experimental. Numerical integration absorption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 2004) |
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 | |
C1 | 0.939 (3) | 0.5104 (17) | 0.7438 (12) | 0.127 (5) | |
H1D | 1.0522 | 0.517 | 0.7507 | 0.152* | |
H1E | 0.8951 | 0.5909 | 0.7035 | 0.152* | |
C2 | 0.888 (3) | 0.3643 (18) | 0.6987 (10) | 0.133 (5) | |
H2A | 0.7759 | 0.3518 | 0.6969 | 0.159* | |
H2B | 0.9412 | 0.283 | 0.7347 | 0.159* | |
C3 | 0.921 (3) | 0.355 (2) | 0.6026 (10) | 0.145 (6) | |
H3A | 0.858 | 0.43 | 0.5657 | 0.174* | |
H3B | 1.0303 | 0.3816 | 0.6043 | 0.174* | |
C4 | 0.892 (3) | 0.207 (2) | 0.5561 (10) | 0.157 (7) | |
H4A | 0.788 | 0.1718 | 0.5622 | 0.189* | |
H4B | 0.9674 | 0.1347 | 0.586 | 0.189* | |
C5 | 0.902 (3) | 0.215 (3) | 0.4558 (9) | 0.146 (8) | |
H5A | 0.8853 | 0.1167 | 0.4292 | 0.22* | |
H5B | 1.0046 | 0.2496 | 0.4494 | 0.22* | |
H5C | 0.8244 | 0.2823 | 0.4253 | 0.22* | |
N1 | 0.8975 (18) | 0.5338 (13) | 0.8290 (8) | 0.097 (4) | |
H1A | 0.9285 | 0.6246 | 0.8493 | 0.145* | |
H1B | 0.9434 | 0.465 | 0.8681 | 0.145* | |
H1C | 0.7939 | 0.5267 | 0.824 | 0.145* | |
I1 | 0.95588 (11) | 0.92510 (9) | 0.78861 (5) | 0.0753 (2) | |
I2 | 0.70034 (8) | 1.21391 (8) | 0.96155 (6) | 0.0662 (2) | |
Pb1 | 1 | 1 | 1 | 0.04330 (15) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.170 (14) | 0.114 (11) | 0.107 (9) | 0.028 (9) | 0.054 (10) | −0.006 (7) |
C2 | 0.170 (13) | 0.130 (10) | 0.098 (8) | 0.036 (10) | 0.026 (9) | −0.021 (7) |
C3 | 0.174 (14) | 0.157 (12) | 0.110 (9) | 0.013 (11) | 0.044 (10) | −0.027 (8) |
C4 | 0.192 (16) | 0.178 (14) | 0.111 (9) | −0.004 (13) | 0.051 (12) | −0.043 (9) |
C5 | 0.159 (17) | 0.183 (19) | 0.093 (9) | −0.046 (15) | 0.011 (11) | −0.030 (10) |
N1 | 0.149 (11) | 0.067 (6) | 0.078 (6) | 0.016 (7) | 0.027 (7) | 0.008 (5) |
I1 | 0.1002 (6) | 0.0647 (5) | 0.0592 (4) | −0.0064 (4) | 0.0094 (4) | −0.0039 (3) |
I2 | 0.0552 (4) | 0.0540 (4) | 0.0922 (5) | 0.0267 (3) | 0.0212 (3) | 0.0083 (3) |
Pb1 | 0.0364 (2) | 0.0325 (2) | 0.0622 (3) | 0.00046 (14) | 0.01189 (18) | −0.00206 (18) |
Geometric parameters (Å, º) top
C1—N1 | 1.394 (19) | C5—H5A | 0.96 |
C1—C2 | 1.499 (9) | C5—H5B | 0.96 |
C1—H1D | 0.97 | C5—H5C | 0.96 |
C1—H1E | 0.97 | N1—H1A | 0.89 |
C2—C3 | 1.511 (9) | N1—H1B | 0.89 |
C2—H2A | 0.97 | N1—H1C | 0.89 |
C2—H2B | 0.97 | I1—Pb1 | 3.1720 (8) |
C3—C4 | 1.498 (9) | I2—Pb1 | 3.1940 (6) |
C3—H3A | 0.97 | I2—Pb1i | 3.1975 (6) |
C3—H3B | 0.97 | Pb1—I1ii | 3.1720 (8) |
C4—C5 | 1.513 (9) | Pb1—I2ii | 3.1940 (6) |
C4—H4A | 0.97 | Pb1—I2iii | 3.1975 (6) |
C4—H4B | 0.97 | Pb1—I2iv | 3.1975 (6) |
| | | |
N1—C1—C2 | 115.7 (14) | H5A—C5—H5B | 109.5 |
N1—C1—H1D | 108.4 | C4—C5—H5C | 109.5 |
C2—C1—H1D | 108.4 | H5A—C5—H5C | 109.5 |
N1—C1—H1E | 108.4 | H5B—C5—H5C | 109.5 |
C2—C1—H1E | 108.4 | C1—N1—H1A | 109.5 |
H1D—C1—H1E | 107.4 | C1—N1—H1B | 109.5 |
C1—C2—C3 | 112.2 (11) | H1A—N1—H1B | 109.5 |
C1—C2—H2A | 109.2 | C1—N1—H1C | 109.5 |
C3—C2—H2A | 109.2 | H1A—N1—H1C | 109.5 |
C1—C2—H2B | 109.2 | H1B—N1—H1C | 109.5 |
C3—C2—H2B | 109.2 | Pb1—I2—Pb1i | 153.68 (3) |
H2A—C2—H2B | 107.9 | I1—Pb1—I1ii | 180 |
C4—C3—C2 | 116.0 (11) | I1—Pb1—I2ii | 90.16 (2) |
C4—C3—H3A | 108.3 | I1ii—Pb1—I2ii | 89.84 (2) |
C2—C3—H3A | 108.3 | I1—Pb1—I2 | 89.84 (2) |
C4—C3—H3B | 108.3 | I1ii—Pb1—I2 | 90.16 (2) |
C2—C3—H3B | 108.3 | I2ii—Pb1—I2 | 180 |
H3A—C3—H3B | 107.4 | I1—Pb1—I2iii | 87.99 (2) |
C3—C4—C5 | 112.3 (12) | I1ii—Pb1—I2iii | 92.01 (2) |
C3—C4—H4A | 109.1 | I2ii—Pb1—I2iii | 93.399 (8) |
C5—C4—H4A | 109.1 | I2—Pb1—I2iii | 86.601 (8) |
C3—C4—H4B | 109.1 | I1—Pb1—I2iv | 92.01 (2) |
C5—C4—H4B | 109.1 | I1ii—Pb1—I2iv | 87.99 (2) |
H4A—C4—H4B | 107.9 | I2ii—Pb1—I2iv | 86.601 (8) |
C4—C5—H5A | 109.5 | I2—Pb1—I2iv | 93.399 (8) |
C4—C5—H5B | 109.5 | I2iii—Pb1—I2iv | 180 |
| | | |
N1—C1—C2—C3 | 173.6 (19) | Pb1i—I2—Pb1—I1ii | 32.34 (6) |
C1—C2—C3—C4 | 173 (2) | Pb1i—I2—Pb1—I2iii | −59.67 (7) |
C2—C3—C4—C5 | 171 (2) | Pb1i—I2—Pb1—I2iv | 120.33 (7) |
Pb1i—I2—Pb1—I1 | −147.66 (6) | | |
Symmetry codes: (i) −x+3/2, y+1/2, −z+2; (ii) −x+2, −y+2, −z+2; (iii) x+1/2, −y+5/2, z; (iv) −x+3/2, y−1/2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I1 | 0.89 | 2.85 | 3.597 (12) | 142 |
N1—H1B···I2v | 0.89 | 2.89 | 3.721 (13) | 156 |
N1—H1C···I1vi | 0.89 | 2.92 | 3.787 (15) | 166 |
Symmetry codes: (v) x+1/2, −y+3/2, z; (vi) x−1/2, −y+3/2, z. |
(2c) bis(pentylammonium)tetraiodoplumbate(II)
top
Crystal data top
2(C5H14N)·I4Pb | F(000) = 1584 |
Mr = 891.13 | Dx = 2.512 Mg m−3 Dm = 0 Mg m−3 Dm measured by not measured |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 4614 reflections |
a = 9.0078 (10) Å | θ = 2.6–28.9° |
b = 8.731 (1) Å | µ = 12.39 mm−1 |
c = 29.956 (4) Å | T = 333 K |
V = 2356.0 (5) Å3 | Plate, red |
Z = 4 | 0.5 × 0.45 × 0.14 mm |
Data collection top
Bruker APEX II CCD area detector diffractometer | 2194 independent reflections |
Radiation source: fine-focus sealed tube | 1566 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.066 |
ω scans | θmax = 25.5°, θmin = 2.6° |
Absorption correction: integration Bruker XPREP (Bruker, 2004) | h = −9→10 |
Tmin = 0.017, Tmax = 0.176 | k = −6→10 |
11216 measured reflections | l = −31→36 |
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)] = 0.124 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.284 | H-atom parameters constrained |
S = 1.32 | w = 1/[σ2(Fo2) + (0.P)2 + 291.1164P] where P = (Fo2 + 2Fc2)/3 |
2194 reflections | (Δ/σ)max = 0.003 |
79 parameters | Δρmax = 2.17 e Å−3 |
48 restraints | Δρmin = −2.67 e Å−3 |
Special details top
Experimental. Numerical integration absorption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 2004) |
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 | |
C1 | 0.973 (8) | 0.468 (9) | 0.894 (2) | 0.27 (2) | |
H1D | 0.8735 | 0.4994 | 0.9025 | 0.326* | |
H1E | 0.9894 | 0.3654 | 0.9052 | 0.326* | |
C2 | 0.986 (7) | 0.469 (11) | 0.843 (2) | 0.28 (2) | |
H2A | 1.007 | 0.5721 | 0.8334 | 0.333* | |
H2B | 1.069 | 0.4045 | 0.8348 | 0.333* | |
C3 | 0.847 (5) | 0.412 (10) | 0.820 (2) | 0.29 (2) | |
H3A | 0.7826 | 0.4984 | 0.814 | 0.342* | |
H3B | 0.7941 | 0.3431 | 0.84 | 0.342* | |
C4 | 0.878 (9) | 0.328 (6) | 0.777 (3) | 0.29 (3) | |
H4A | 0.9555 | 0.2528 | 0.7816 | 0.347* | |
H4B | 0.7896 | 0.2745 | 0.7672 | 0.347* | |
C5 | 0.927 (11) | 0.435 (10) | 0.739 (2) | 0.30 (3) | |
H5A | 0.9098 | 0.3869 | 0.7109 | 0.45* | |
H5B | 1.0313 | 0.457 | 0.7423 | 0.45* | |
H5C | 0.8718 | 0.5288 | 0.7409 | 0.45* | |
N1 | 1.080 (6) | 0.572 (7) | 0.914 (2) | 0.25 (3) | |
H1A | 1.0679 | 0.5735 | 0.9432 | 0.375* | |
H1B | 1.0672 | 0.6654 | 0.9027 | 0.375* | |
H1C | 1.1716 | 0.5395 | 0.9074 | 0.375* | |
I1 | 1.0425 (4) | 0.9841 (4) | 0.89404 (13) | 0.1034 (12) | |
I2 | 0.7090 (3) | 1.2066 (3) | 0.99199 (13) | 0.0927 (11) | |
Pb1 | 1 | 1 | 1 | 0.0610 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.15 (4) | 0.20 (4) | 0.46 (7) | −0.05 (3) | 0.11 (4) | −0.03 (5) |
C2 | 0.17 (4) | 0.20 (4) | 0.46 (7) | −0.05 (3) | 0.10 (5) | −0.02 (5) |
C3 | 0.18 (4) | 0.21 (4) | 0.47 (7) | −0.05 (3) | 0.10 (5) | −0.03 (5) |
C4 | 0.19 (4) | 0.21 (5) | 0.46 (7) | −0.05 (3) | 0.09 (5) | −0.03 (5) |
C5 | 0.22 (5) | 0.21 (5) | 0.46 (7) | −0.06 (5) | 0.09 (5) | −0.02 (5) |
N1 | 0.11 (4) | 0.19 (5) | 0.46 (7) | −0.02 (3) | 0.11 (4) | −0.02 (5) |
I1 | 0.099 (2) | 0.104 (3) | 0.108 (3) | 0.019 (2) | −0.0040 (19) | 0.009 (2) |
I2 | 0.0608 (15) | 0.0622 (16) | 0.155 (3) | 0.0314 (13) | −0.0187 (18) | −0.011 (2) |
Pb1 | 0.0358 (8) | 0.0403 (9) | 0.1069 (17) | 0.0003 (8) | 0.0014 (10) | 0.0057 (13) |
Geometric parameters (Å, º) top
C1—N1 | 1.449 (10) | C5—H5A | 0.96 |
C1—C2 | 1.520 (10) | C5—H5B | 0.96 |
C1—H1D | 0.97 | C5—H5C | 0.96 |
C1—H1E | 0.97 | N1—H1A | 0.89 |
C2—C3 | 1.518 (10) | N1—H1B | 0.89 |
C2—H2A | 0.97 | N1—H1C | 0.89 |
C2—H2B | 0.97 | I1—Pb1 | 3.200 (4) |
C3—C4 | 1.520 (10) | I2—Pb1i | 3.188 (2) |
C3—H3A | 0.97 | I2—Pb1 | 3.191 (2) |
C3—H3B | 0.97 | Pb1—I2ii | 3.188 (2) |
C4—C5 | 1.519 (10) | Pb1—I2iii | 3.188 (2) |
C4—H4A | 0.97 | Pb1—I2iv | 3.191 (2) |
C4—H4B | 0.97 | Pb1—I1iv | 3.200 (4) |
| | | |
N1—C1—C2 | 110.7 (16) | H5A—C5—H5B | 109.5 |
N1—C1—H1D | 109.5 | C4—C5—H5C | 109.5 |
C2—C1—H1D | 109.5 | H5A—C5—H5C | 109.5 |
N1—C1—H1E | 109.5 | H5B—C5—H5C | 109.5 |
C2—C1—H1E | 109.5 | C1—N1—H1A | 109.5 |
H1D—C1—H1E | 108.1 | C1—N1—H1B | 109.5 |
C3—C2—C1 | 113.2 (16) | H1A—N1—H1B | 109.5 |
C3—C2—H2A | 108.9 | C1—N1—H1C | 109.5 |
C1—C2—H2A | 108.9 | H1A—N1—H1C | 109.5 |
C3—C2—H2B | 108.9 | H1B—N1—H1C | 109.5 |
C1—C2—H2B | 108.9 | Pb1i—I2—Pb1 | 159.01 (11) |
H2A—C2—H2B | 107.8 | I2ii—Pb1—I2iii | 180 |
C2—C3—C4 | 113.4 (16) | I2ii—Pb1—I2iv | 92.095 (19) |
C2—C3—H3A | 108.9 | I2iii—Pb1—I2iv | 87.91 (2) |
C4—C3—H3A | 108.9 | I2ii—Pb1—I2 | 87.91 (2) |
C2—C3—H3B | 108.9 | I2iii—Pb1—I2 | 92.095 (19) |
C4—C3—H3B | 108.9 | I2iv—Pb1—I2 | 180.00 (14) |
H3A—C3—H3B | 107.7 | I2ii—Pb1—I1iv | 92.23 (10) |
C5—C4—C3 | 113.1 (16) | I2iii—Pb1—I1iv | 87.77 (10) |
C5—C4—H4A | 109 | I2iv—Pb1—I1iv | 92.76 (9) |
C3—C4—H4A | 109 | I2—Pb1—I1iv | 87.24 (9) |
C5—C4—H4B | 109 | I2ii—Pb1—I1 | 87.77 (10) |
C3—C4—H4B | 109 | I2iii—Pb1—I1 | 92.23 (10) |
H4A—C4—H4B | 107.8 | I2iv—Pb1—I1 | 87.24 (9) |
C4—C5—H5A | 109.5 | I2—Pb1—I1 | 92.76 (9) |
C4—C5—H5B | 109.5 | I1iv—Pb1—I1 | 180.0000 (10) |
| | | |
N1—C1—C2—C3 | −159 (7) | Pb1i—I2—Pb1—I2iii | −19.9 (3) |
C1—C2—C3—C4 | −148 (7) | Pb1i—I2—Pb1—I1iv | 67.8 (4) |
C2—C3—C4—C5 | −72 (8) | Pb1i—I2—Pb1—I1 | −112.2 (4) |
Pb1i—I2—Pb1—I2ii | 160.1 (3) | | |
Symmetry codes: (i) x−1/2, −y+5/2, −z+2; (ii) −x+3/2, y−1/2, z; (iii) x+1/2, −y+5/2, −z+2; (iv) −x+2, −y+2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I2ii | 0.89 | 3.12 | 3.70 (5) | 125 |
N1—H1B···I1 | 0.89 | 2.8 | 3.66 (7) | 163 |
N1—H1C···I1v | 0.89 | 2.65 | 3.53 (5) | 171 |
Symmetry codes: (ii) −x+3/2, y−1/2, z; (v) −x+5/2, y−1/2, z. |
(3a) bis(hexylammonium)tetraiodoplumbate(II)
top
Crystal data top
2(C6H16N)·I4Pb | F(000) = 824 |
Mr = 919.19 | Dx = 2.489 Mg m−3 |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yab | Cell parameters from 866 reflections |
a = 8.643 (4) Å | θ = 6.6–56.4° |
b = 8.845 (4) Å | µ = 11.91 mm−1 |
c = 16.052 (7) Å | T = 173 K |
β = 91.985 (8)° | Plate, yellow |
V = 1226.4 (10) Å3 | 0.32 × 0.16 × 0.02 mm |
Z = 2 | |
Data collection top
Bruker APEX II CCD area detector diffractometer | 2984 independent reflections |
Radiation source: fine-focus sealed tube | 2563 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.092 |
ω scans | θmax = 28°, θmin = 1.3° |
Absorption correction: integration Bruker XPREP (Bruker, 2004) | h = −11→11 |
Tmin = 0.147, Tmax = 0.784 | k = −11→11 |
11777 measured reflections | l = −18→21 |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.143 | H-atom parameters constrained |
S = 1.21 | w = 1/[σ2(Fo2) + (0.0221P)2 + 49.3157P] where P = (Fo2 + 2Fc2)/3 |
2984 reflections | (Δ/σ)max = 0.002 |
89 parameters | Δρmax = 4.93 e Å−3 |
0 restraints | Δρmin = −2.77 e Å−3 |
Special details top
Experimental. Numerical integration absorption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 2004) |
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 | |
C1 | 0.9621 (18) | 0.4637 (18) | 0.8019 (11) | 0.035 (4) | |
H1D | 0.8616 | 0.4728 | 0.8293 | 0.041* | |
H1E | 1.0015 | 0.3598 | 0.8115 | 0.041* | |
C2 | 0.939 (2) | 0.490 (2) | 0.7102 (11) | 0.042 (4) | |
H2A | 1.0403 | 0.4871 | 0.6836 | 0.05* | |
H2B | 0.8946 | 0.5926 | 0.7011 | 0.05* | |
C3 | 0.831 (2) | 0.3738 (18) | 0.6686 (10) | 0.035 (4) | |
H3A | 0.8822 | 0.2735 | 0.6698 | 0.042* | |
H3B | 0.735 | 0.366 | 0.7 | 0.042* | |
C4 | 0.791 (2) | 0.417 (2) | 0.5793 (11) | 0.043 (4) | |
H4A | 0.8874 | 0.4225 | 0.5479 | 0.051* | |
H4B | 0.7427 | 0.5181 | 0.5783 | 0.051* | |
C5 | 0.681 (3) | 0.305 (2) | 0.5363 (12) | 0.049 (5) | |
H5A | 0.5848 | 0.2986 | 0.5677 | 0.059* | |
H5B | 0.7295 | 0.2031 | 0.5374 | 0.059* | |
C6 | 0.640 (3) | 0.347 (3) | 0.4462 (13) | 0.066 (7) | |
H6A | 0.5689 | 0.2724 | 0.4217 | 0.098* | |
H6B | 0.7349 | 0.3504 | 0.4142 | 0.098* | |
H6C | 0.5911 | 0.4473 | 0.4447 | 0.098* | |
N1 | 1.0710 (16) | 0.5717 (15) | 0.8387 (10) | 0.037 (3) | |
H1A | 1.0832 | 0.5534 | 0.8943 | 0.056* | |
H1B | 1.0342 | 0.6671 | 0.8306 | 0.056* | |
H1C | 1.1639 | 0.5622 | 0.8142 | 0.056* | |
I1 | 0.97165 (12) | 0.96748 (11) | 0.80108 (6) | 0.0293 (2) | |
I2 | 0.69394 (10) | 1.19584 (10) | 0.99643 (6) | 0.0250 (2) | |
Pb1 | 1 | 1 | 1 | 0.01592 (17) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.020 (7) | 0.032 (8) | 0.051 (10) | 0.012 (6) | −0.007 (7) | −0.003 (7) |
C2 | 0.057 (12) | 0.036 (9) | 0.032 (9) | −0.008 (8) | −0.006 (8) | 0.008 (7) |
C3 | 0.045 (9) | 0.028 (8) | 0.032 (8) | −0.004 (7) | −0.006 (7) | 0.004 (6) |
C4 | 0.056 (11) | 0.042 (9) | 0.030 (9) | 0.009 (8) | −0.003 (8) | 0.007 (7) |
C5 | 0.065 (13) | 0.046 (11) | 0.035 (10) | −0.003 (9) | −0.009 (9) | −0.002 (8) |
C6 | 0.093 (19) | 0.065 (14) | 0.036 (11) | 0.012 (13) | −0.018 (11) | −0.012 (10) |
N1 | 0.032 (7) | 0.028 (7) | 0.050 (9) | −0.004 (6) | −0.014 (6) | 0.013 (6) |
I1 | 0.0374 (5) | 0.0256 (5) | 0.0248 (5) | 0.0015 (4) | 0.0011 (4) | 0.0039 (4) |
I2 | 0.0176 (4) | 0.0197 (4) | 0.0376 (5) | 0.0079 (3) | −0.0024 (3) | −0.0052 (3) |
Pb1 | 0.0119 (3) | 0.0118 (3) | 0.0240 (4) | −0.0003 (2) | −0.0002 (2) | 0.0001 (3) |
Geometric parameters (Å, º) top
C1—N1 | 1.45 (2) | C5—H5B | 0.99 |
C1—C2 | 1.50 (2) | C6—H6A | 0.98 |
C1—H1D | 0.99 | C6—H6B | 0.98 |
C1—H1E | 0.99 | C6—H6C | 0.98 |
C2—C3 | 1.53 (2) | N1—H1A | 0.91 |
C2—H2A | 0.99 | N1—H1B | 0.91 |
C2—H2B | 0.99 | N1—H1C | 0.91 |
C3—C4 | 1.51 (2) | I1—Pb1 | 3.2069 (17) |
C3—H3A | 0.99 | I2—Pb1 | 3.1608 (13) |
C3—H3B | 0.99 | I2—Pb1i | 3.1712 (13) |
C4—C5 | 1.52 (3) | Pb1—I2ii | 3.1608 (13) |
C4—H4A | 0.99 | Pb1—I2iii | 3.1712 (14) |
C4—H4B | 0.99 | Pb1—I2iv | 3.1712 (14) |
C5—C6 | 1.53 (3) | Pb1—I1ii | 3.2069 (17) |
C5—H5A | 0.99 | | |
| | | |
N1—C1—C2 | 111.1 (15) | H5A—C5—H5B | 107.8 |
N1—C1—H1D | 109.4 | C5—C6—H6A | 109.5 |
C2—C1—H1D | 109.4 | C5—C6—H6B | 109.5 |
N1—C1—H1E | 109.4 | H6A—C6—H6B | 109.5 |
C2—C1—H1E | 109.4 | C5—C6—H6C | 109.5 |
H1D—C1—H1E | 108 | H6A—C6—H6C | 109.5 |
C1—C2—C3 | 112.5 (14) | H6B—C6—H6C | 109.5 |
C1—C2—H2A | 109.1 | C1—N1—H1A | 109.5 |
C3—C2—H2A | 109.1 | C1—N1—H1B | 109.5 |
C1—C2—H2B | 109.1 | H1A—N1—H1B | 109.5 |
C3—C2—H2B | 109.1 | C1—N1—H1C | 109.5 |
H2A—C2—H2B | 107.8 | H1A—N1—H1C | 109.5 |
C4—C3—C2 | 111.2 (14) | H1B—N1—H1C | 109.5 |
C4—C3—H3A | 109.4 | Pb1—I2—Pb1i | 155.11 (3) |
C2—C3—H3A | 109.4 | I2ii—Pb1—I2 | 180 |
C4—C3—H3B | 109.4 | I2ii—Pb1—I2iii | 88.70 (3) |
C2—C3—H3B | 109.4 | I2—Pb1—I2iii | 91.30 (3) |
H3A—C3—H3B | 108 | I2ii—Pb1—I2iv | 91.30 (3) |
C3—C4—C5 | 112.7 (15) | I2—Pb1—I2iv | 88.70 (3) |
C3—C4—H4A | 109 | I2iii—Pb1—I2iv | 180 |
C5—C4—H4A | 109 | I2ii—Pb1—I1 | 90.22 (3) |
C3—C4—H4B | 109 | I2—Pb1—I1 | 89.78 (3) |
C5—C4—H4B | 109 | I2iii—Pb1—I1 | 85.39 (3) |
H4A—C4—H4B | 107.8 | I2iv—Pb1—I1 | 94.61 (3) |
C4—C5—C6 | 112.9 (18) | I2ii—Pb1—I1ii | 89.78 (3) |
C4—C5—H5A | 109 | I2—Pb1—I1ii | 90.22 (3) |
C6—C5—H5A | 109 | I2iii—Pb1—I1ii | 94.61 (3) |
C4—C5—H5B | 109 | I2iv—Pb1—I1ii | 85.39 (3) |
C6—C5—H5B | 109 | I1—Pb1—I1ii | 180 |
| | | |
N1—C1—C2—C3 | 177.0 (15) | Pb1i—I2—Pb1—I2iii | 174.29 (10) |
C1—C2—C3—C4 | 171.6 (16) | Pb1i—I2—Pb1—I2iv | −5.71 (10) |
C2—C3—C4—C5 | −178.8 (17) | Pb1i—I2—Pb1—I1 | −100.32 (9) |
C3—C4—C5—C6 | 180.0 (18) | Pb1i—I2—Pb1—I1ii | 79.68 (9) |
Symmetry codes: (i) −x+3/2, y+1/2, −z+2; (ii) −x+2, −y+2, −z+2; (iii) −x+3/2, y−1/2, −z+2; (iv) x+1/2, −y+5/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I2v | 0.91 | 2.89 | 3.599 (13) | 136 |
N1—H1B···I1 | 0.91 | 2.75 | 3.650 (13) | 171 |
N1—H1C···I1v | 0.91 | 2.69 | 3.553 (15) | 159 |
Symmetry code: (v) x+1/2, −y+3/2, z. |
(3b) bis(hexylammonium)tetraiodoplumbate(II)
top
Crystal data top
2(C6H16N)·I4Pb | F(000) = 1648 |
Mr = 919.19 | Dx = 2.403 Mg m−3 Dm = 0 Mg m−3 Dm measured by not measured |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 5270 reflections |
a = 8.9413 (2) Å | θ = 2.6–29.9° |
b = 8.6874 (2) Å | µ = 11.50 mm−1 |
c = 32.7027 (10) Å | T = 293 K |
V = 2540.24 (11) Å3 | Plate, orange |
Z = 4 | 0.46 × 0.28 × 0.05 mm |
Data collection top
Bruker APEX II CCD area detector diffractometer | 3056 independent reflections |
Radiation source: fine-focus sealed tube | 2421 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
ω scans | θmax = 28°, θmin = 2.6° |
Absorption correction: integration Bruker XPREP (Bruker, 2004) | h = −9→11 |
Tmin = 0.058, Tmax = 0.536 | k = −10→11 |
12552 measured reflections | l = −42→43 |
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)] = 0.081 | H-atom parameters constrained |
wR(F2) = 0.168 | w = 1/[σ2(Fo2) + (0.P)2 + 101.7161P] where P = (Fo2 + 2Fc2)/3 |
S = 1.34 | (Δ/σ)max < 0.001 |
3056 reflections | Δρmax = 1.65 e Å−3 |
89 parameters | Δρmin = −1.69 e Å−3 |
56 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00037 (4) |
Special details top
Experimental. Numerical integration absorption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 2004) |
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 | |
C1 | 0.970 (4) | 0.463 (4) | 0.9038 (6) | 0.120 (8) | |
H1D | 0.8689 | 0.4845 | 0.913 | 0.144* | |
H1E | 0.9957 | 0.358 | 0.9111 | 0.144* | |
C2 | 0.985 (4) | 0.489 (4) | 0.8585 (6) | 0.136 (8) | |
H2A | 1.0882 | 0.4693 | 0.8508 | 0.163* | |
H2B | 0.9647 | 0.5967 | 0.8528 | 0.163* | |
C3 | 0.883 (4) | 0.391 (4) | 0.8320 (6) | 0.148 (8) | |
H3A | 0.7796 | 0.4145 | 0.8379 | 0.177* | |
H3B | 0.8999 | 0.2824 | 0.8379 | 0.177* | |
C4 | 0.917 (4) | 0.423 (4) | 0.7872 (6) | 0.164 (9) | |
H4A | 0.8935 | 0.5296 | 0.7813 | 0.197* | |
H4B | 1.0236 | 0.409 | 0.7825 | 0.197* | |
C5 | 0.832 (4) | 0.321 (4) | 0.7578 (7) | 0.177 (10) | |
H5A | 0.7256 | 0.3351 | 0.762 | 0.213* | |
H5B | 0.8561 | 0.2144 | 0.7632 | 0.213* | |
C6 | 0.871 (5) | 0.360 (5) | 0.7136 (7) | 0.202 (15) | |
H6A | 0.8147 | 0.294 | 0.6956 | 0.303* | |
H6B | 0.9758 | 0.3435 | 0.7091 | 0.303* | |
H6C | 0.8463 | 0.4652 | 0.7081 | 0.303* | |
N1 | 1.078 (2) | 0.574 (2) | 0.9216 (7) | 0.086 (5) | |
H1A | 1.0749 | 0.5688 | 0.9488 | 0.129* | |
H1B | 1.055 | 0.6691 | 0.9136 | 0.129* | |
H1C | 1.1703 | 0.5512 | 0.9131 | 0.129* | |
I1 | 1.03252 (17) | 0.98288 (17) | 0.90247 (5) | 0.0689 (4) | |
I2 | 0.69807 (13) | 1.19581 (14) | 0.99628 (5) | 0.0637 (4) | |
Pb1 | 1 | 1 | 1 | 0.0443 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.112 (16) | 0.122 (17) | 0.127 (12) | −0.016 (13) | −0.005 (15) | −0.027 (16) |
C2 | 0.137 (17) | 0.145 (18) | 0.126 (12) | 0.005 (15) | −0.008 (14) | −0.028 (15) |
C3 | 0.149 (18) | 0.164 (19) | 0.130 (12) | 0.012 (17) | −0.022 (15) | −0.035 (16) |
C4 | 0.17 (2) | 0.19 (2) | 0.129 (12) | 0.02 (2) | −0.022 (16) | −0.032 (17) |
C5 | 0.18 (2) | 0.22 (2) | 0.132 (14) | 0.02 (2) | −0.029 (18) | −0.041 (19) |
C6 | 0.22 (3) | 0.26 (4) | 0.126 (13) | 0.05 (3) | −0.03 (2) | −0.03 (2) |
N1 | 0.057 (10) | 0.082 (13) | 0.120 (13) | 0.016 (9) | −0.003 (10) | −0.003 (11) |
I1 | 0.0759 (9) | 0.0620 (8) | 0.0687 (9) | 0.0080 (8) | −0.0078 (7) | 0.0020 (7) |
I2 | 0.0451 (6) | 0.0439 (6) | 0.1019 (11) | 0.0175 (5) | −0.0117 (7) | −0.0073 (7) |
Pb1 | 0.0328 (4) | 0.0322 (4) | 0.0679 (6) | 0.0001 (3) | −0.0003 (4) | 0.0003 (5) |
Geometric parameters (Å, º) top
C1—N1 | 1.49 (3) | C5—H5B | 0.97 |
C1—C2 | 1.504 (10) | C6—H6A | 0.96 |
C1—H1D | 0.97 | C6—H6B | 0.96 |
C1—H1E | 0.97 | C6—H6C | 0.96 |
C2—C3 | 1.522 (10) | N1—H1A | 0.89 |
C2—H2A | 0.97 | N1—H1B | 0.89 |
C2—H2B | 0.97 | N1—H1C | 0.89 |
C3—C4 | 1.525 (10) | I1—Pb1 | 3.2062 (15) |
C3—H3A | 0.97 | I2—Pb1i | 3.1835 (11) |
C3—H3B | 0.97 | I2—Pb1 | 3.1932 (11) |
C4—C5 | 1.510 (10) | Pb1—I2ii | 3.1835 (11) |
C4—H4A | 0.97 | Pb1—I2iii | 3.1835 (11) |
C4—H4B | 0.97 | Pb1—I2iv | 3.1932 (11) |
C5—C6 | 1.523 (10) | Pb1—I1iv | 3.2062 (15) |
C5—H5A | 0.97 | | |
| | | |
N1—C1—C2 | 103 (2) | H5A—C5—H5B | 108 |
N1—C1—H1D | 111.1 | C5—C6—H6A | 109.5 |
C2—C1—H1D | 111.1 | C5—C6—H6B | 109.5 |
N1—C1—H1E | 111.1 | H6A—C6—H6B | 109.5 |
C2—C1—H1E | 111.1 | C5—C6—H6C | 109.5 |
H1D—C1—H1E | 109.1 | H6A—C6—H6C | 109.5 |
C1—C2—C3 | 114.9 (14) | H6B—C6—H6C | 109.5 |
C1—C2—H2A | 108.5 | C1—N1—H1A | 109.5 |
C3—C2—H2A | 108.5 | C1—N1—H1B | 109.5 |
C1—C2—H2B | 108.5 | H1A—N1—H1B | 109.5 |
C3—C2—H2B | 108.5 | C1—N1—H1C | 109.5 |
H2A—C2—H2B | 107.5 | H1A—N1—H1C | 109.5 |
C2—C3—C4 | 109.0 (13) | H1B—N1—H1C | 109.5 |
C2—C3—H3A | 109.9 | Pb1i—I2—Pb1 | 155.65 (5) |
C4—C3—H3A | 109.9 | I2ii—Pb1—I2iii | 180 |
C2—C3—H3B | 109.9 | I2ii—Pb1—I2iv | 91.695 (9) |
C4—C3—H3B | 109.9 | I2iii—Pb1—I2iv | 88.305 (9) |
H3A—C3—H3B | 108.3 | I2ii—Pb1—I2 | 88.305 (9) |
C5—C4—C3 | 113.8 (14) | I2iii—Pb1—I2 | 91.695 (9) |
C5—C4—H4A | 108.8 | I2iv—Pb1—I2 | 180.0000 (10) |
C3—C4—H4A | 108.8 | I2ii—Pb1—I1iv | 91.50 (4) |
C5—C4—H4B | 108.8 | I2iii—Pb1—I1iv | 88.50 (4) |
C3—C4—H4B | 108.8 | I2iv—Pb1—I1iv | 93.64 (4) |
H4A—C4—H4B | 107.7 | I2—Pb1—I1iv | 86.36 (4) |
C4—C5—C6 | 111.2 (14) | I2ii—Pb1—I1 | 88.50 (4) |
C4—C5—H5A | 109.4 | I2iii—Pb1—I1 | 91.50 (4) |
C6—C5—H5A | 109.4 | I2iv—Pb1—I1 | 86.36 (4) |
C4—C5—H5B | 109.4 | I2—Pb1—I1 | 93.64 (4) |
C6—C5—H5B | 109.4 | I1iv—Pb1—I1 | 180.0000 (10) |
| | | |
N1—C1—C2—C3 | −179 (3) | Pb1i—I2—Pb1—I2ii | 171.92 (11) |
C1—C2—C3—C4 | −177 (3) | Pb1i—I2—Pb1—I2iii | −8.08 (11) |
C2—C3—C4—C5 | 175 (3) | Pb1i—I2—Pb1—I1iv | 80.32 (14) |
C3—C4—C5—C6 | 180 (4) | Pb1i—I2—Pb1—I1 | −99.68 (14) |
Symmetry codes: (i) x−1/2, −y+5/2, −z+2; (ii) −x+3/2, y−1/2, z; (iii) x+1/2, −y+5/2, −z+2; (iv) −x+2, −y+2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I2ii | 0.89 | 3.1 | 3.63 (2) | 121 |
N1—H1B···I1 | 0.89 | 2.76 | 3.63 (2) | 166 |
N1—H1C···I1v | 0.89 | 2.74 | 3.622 (18) | 169 |
Symmetry codes: (ii) −x+3/2, y−1/2, z; (v) −x+5/2, y−1/2, z. |