Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106014417/fg3016sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270106014417/fg3016Isup2.hkl |
CCDC reference: 612437
PbI2 (0.092 g, 0.200 mmol) was dissolved in 47% HI (2 ml) in a sample vial. C3H7NH2 (0.026 g, 0.427 mmol) was added and the precipitate was dissolved by refluxing for 2 h at 363 K. The solution was cooled slowly at 2 K h−1 to room temperature. A yellow single-crystal suitable for X-ray diffraction analysis was selected and studied. Analysis calculated for C24H80I18N8Pb5: C 7.58, H 2.12, N 2.95%; found: C 7.63, H 2.27, N 3.04%
H atoms bonded to C and N atoms were refined in idealized positions in the riding-model approximation, with C—H distances of 0.98 Å and 0.99 Å for methyl and methylene H atoms, respectively, N—H distances of 0.91 Å, and Uiso(H) values of 1.2Ueq(C) (for CH2) or Uiso(H) = 1.5Ueq(C,N) for CH3 and NH3. The conformational disorder around cations cat4, cat5 and cat6 was resolved by finding alternate [alternative?] positions from the difference Fourier map for all C and N atoms that make up the propylammonium chains. These atoms were then refined anisotropically together with their site occupancy such that the sum of the occupancies for the two chains equaled one. H-atom positions were then calculated for the respective atoms using a riding model as above. For cat4, the major to minor ratio was 60:40%. For cat5, the major to minor ratio was 57:43%. For cat6, the major to minor ratio was 54:46%.
Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999) and PLATON (Spek, 2002).
(C3H10N)8[Pb5I18] | F(000) = 6576 |
Mr = 3801.11 | Dx = 3.181 Mg m−3 |
Monoclinic, P2/c | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -P 2yc | Cell parameters from 962 reflections |
a = 23.988 (5) Å | θ = 2.5–27.9° |
b = 8.754 (5) Å | µ = 17.60 mm−1 |
c = 37.986 (5) Å | T = 173 K |
β = 95.718 (5)° | Needle, yellow |
V = 7937 (5) Å3 | 0.44 × 0.06 × 0.06 mm |
Z = 4 |
Bruker SMART-NT CCD area-detector diffractometer | 9140 reflections with I > 2σ(I) |
ϕ and ω scans | Rint = 0.090 |
Absorption correction: integration (XPREP; Bruker, 1999) | θmax = 25°, θmin = 0.9° |
Tmin = 0.076, Tmax = 0.392 | h = −24→28 |
52039 measured reflections | k = −10→10 |
13878 independent reflections | l = −43→45 |
Refinement on F2 | 470 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.045 | w = 1/[σ2(Fo2) + (0.0483P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.108 | (Δ/σ)max = 0.004 |
S = 1.00 | Δρmax = 2.21 e Å−3 |
13878 reflections | Δρmin = −1.85 e Å−3 |
625 parameters |
(C3H10N)8[Pb5I18] | V = 7937 (5) Å3 |
Mr = 3801.11 | Z = 4 |
Monoclinic, P2/c | Mo Kα radiation |
a = 23.988 (5) Å | µ = 17.60 mm−1 |
b = 8.754 (5) Å | T = 173 K |
c = 37.986 (5) Å | 0.44 × 0.06 × 0.06 mm |
β = 95.718 (5)° |
Bruker SMART-NT CCD area-detector diffractometer | 13878 independent reflections |
Absorption correction: integration (XPREP; Bruker, 1999) | 9140 reflections with I > 2σ(I) |
Tmin = 0.076, Tmax = 0.392 | Rint = 0.090 |
52039 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | 470 restraints |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 1.00 | Δρmax = 2.21 e Å−3 |
13878 reflections | Δρmin = −1.85 e Å−3 |
625 parameters |
Experimental. Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pb1 | 0.12858 (2) | 0.53869 (5) | 0.189953 (14) | 0.02095 (13) | |
Pb2 | 0.32761 (3) | 1.01583 (5) | 0.225907 (15) | 0.02229 (14) | |
Pb3 | 0.37147 (2) | 1.02190 (5) | 0.059913 (15) | 0.02104 (14) | |
Pb4 | 0.17127 (2) | 0.54071 (6) | 0.023102 (15) | 0.02296 (14) | |
Pb5 | 0 | 0.55044 (8) | 0.25 | 0.0265 (2) | |
Pb6 | 0.5 | 1 | 0 | 0.0273 (2) | |
I1 | 0.22551 (4) | 0.28129 (9) | 0.20077 (3) | 0.0273 (2) | |
I2 | 0.03360 (4) | 0.79559 (9) | 0.19272 (3) | 0.0294 (2) | |
I3 | 0.03641 (4) | 0.28668 (10) | 0.19717 (3) | 0.0322 (2) | |
I4 | 0.13355 (5) | 0.57536 (11) | 0.27387 (3) | 0.0383 (3) | |
I5 | 0.22974 (5) | 0.77966 (10) | 0.18788 (3) | 0.0322 (2) | |
I6 | 0.28052 (5) | 0.94181 (12) | 0.29635 (3) | 0.0393 (3) | |
I7 | 0.41460 (4) | 0.76745 (9) | 0.24213 (3) | 0.0295 (2) | |
I8 | 0.41013 (4) | 1.27435 (10) | 0.25040 (3) | 0.0321 (2) | |
I9 | 0.36487 (5) | 1.05883 (12) | 0.14314 (3) | 0.0414 (3) | |
I10 | 0.46805 (5) | 0.77270 (10) | 0.06166 (3) | 0.0345 (3) | |
I11 | 0.36718 (5) | 0.96300 (11) | −0.02372 (3) | 0.0380 (3) | |
I12 | 0.46384 (4) | 1.27576 (9) | 0.04960 (3) | 0.0305 (2) | |
I13 | 0.27341 (4) | 1.27657 (9) | 0.04812 (3) | 0.0273 (2) | |
I14 | 0.27048 (4) | 0.77968 (10) | 0.06092 (3) | 0.0305 (2) | |
I15 | 0.21673 (5) | 0.60562 (12) | −0.04815 (3) | 0.0411 (3) | |
I16 | 0.08094 (4) | 0.78033 (10) | 0.00680 (3) | 0.0317 (2) | |
I17 | 0.09291 (4) | 0.27338 (10) | −0.00052 (3) | 0.0301 (2) | |
I18 | 0.13539 (5) | 0.49707 (12) | 0.10627 (3) | 0.0401 (3) | |
N1 | 0.1978 (6) | 1.0576 (14) | 0.1152 (4) | 0.044 (3) | |
H1A | 0.199 | 1.1578 | 0.1216 | 0.067* | |
H1B | 0.2257 | 1.0379 | 0.1013 | 0.067* | |
H1C | 0.2025 | 0.9982 | 0.135 | 0.067* | |
C11 | 0.1423 (7) | 1.023 (2) | 0.0951 (5) | 0.054 (4) | |
H11A | 0.1351 | 1.0974 | 0.0756 | 0.065* | |
H11B | 0.1437 | 0.9198 | 0.0845 | 0.065* | |
C12 | 0.0971 (7) | 1.029 (2) | 0.1173 (5) | 0.061 (4) | |
H12A | 0.0981 | 1.1275 | 0.13 | 0.073* | |
H12B | 0.102 | 0.9462 | 0.1352 | 0.073* | |
C13 | 0.0433 (10) | 1.011 (2) | 0.0969 (7) | 0.072 (6) | |
H13A | 0.0449 | 1.0566 | 0.0734 | 0.107* | |
H13B | 0.0145 | 1.0633 | 0.109 | 0.107* | |
H13C | 0.0341 | 0.9026 | 0.0944 | 0.107* | |
N2 | 0.2985 (7) | 0.4987 (14) | 0.1331 (4) | 0.048 (4) | |
H2A | 0.2951 | 0.5677 | 0.1151 | 0.072* | |
H2B | 0.2704 | 0.5133 | 0.1472 | 0.072* | |
H2C | 0.2963 | 0.4024 | 0.124 | 0.072* | |
C21 | 0.3540 (7) | 0.520 (2) | 0.1545 (5) | 0.056 (4) | |
H21A | 0.354 | 0.6184 | 0.1673 | 0.068* | |
H21B | 0.3596 | 0.4372 | 0.1722 | 0.068* | |
C22 | 0.4004 (7) | 0.518 (2) | 0.1319 (6) | 0.058 (4) | |
H22A | 0.3956 | 0.6048 | 0.1151 | 0.07* | |
H22B | 0.3986 | 0.4227 | 0.118 | 0.07* | |
C23 | 0.4562 (9) | 0.530 (2) | 0.1520 (7) | 0.081 (7) | |
H23A | 0.4627 | 0.6354 | 0.16 | 0.121* | |
H23B | 0.485 | 0.5002 | 0.1367 | 0.121* | |
H23C | 0.4579 | 0.4619 | 0.1725 | 0.121* | |
N3 | 0.4988 (6) | 1.0211 (13) | 0.3072 (4) | 0.040 (3) | |
H3A | 0.4827 | 1.0933 | 0.2923 | 0.06* | |
H3B | 0.5055 | 0.9354 | 0.2947 | 0.06* | |
H3C | 0.5318 | 1.0574 | 0.318 | 0.06* | |
C31 | 0.4602 (8) | 0.9833 (18) | 0.3347 (5) | 0.052 (4) | |
H31A | 0.4253 | 0.9387 | 0.3229 | 0.062* | |
H31B | 0.4782 | 0.9055 | 0.351 | 0.062* | |
C32 | 0.4461 (9) | 1.120 (2) | 0.3555 (5) | 0.061 (5) | |
H32A | 0.4813 | 1.165 | 0.3668 | 0.073* | |
H32B | 0.428 | 1.197 | 0.339 | 0.073* | |
C33 | 0.4083 (9) | 1.087 (3) | 0.3834 (5) | 0.077 (6) | |
H33A | 0.3751 | 1.0324 | 0.373 | 0.115* | |
H33B | 0.3968 | 1.1837 | 0.3937 | 0.115* | |
H33C | 0.4282 | 1.0244 | 0.402 | 0.115* | |
N4A | 0.205 (3) | 1.007 (10) | −0.0206 (12) | 0.033 (8) | 0.60 (2) |
H4AA | 0.2103 | 0.9098 | −0.0284 | 0.049* | 0.60 (2) |
H4AB | 0.1682 | 1.0196 | −0.0172 | 0.049* | 0.60 (2) |
H4AC | 0.2266 | 1.0219 | 0.0001 | 0.049* | 0.60 (2) |
C41A | 0.2203 (13) | 1.115 (3) | −0.0466 (6) | 0.042 (5) | 0.60 (2) |
H41A | 0.2614 | 1.1106 | −0.0474 | 0.05* | 0.60 (2) |
H41B | 0.2107 | 1.2188 | −0.039 | 0.05* | 0.60 (2) |
C42A | 0.1927 (15) | 1.088 (3) | −0.0827 (6) | 0.054 (6) | 0.60 (2) |
H42A | 0.1525 | 1.1137 | −0.0828 | 0.064* | 0.60 (2) |
H42B | 0.1951 | 0.9773 | −0.088 | 0.064* | 0.60 (2) |
C43A | 0.216 (2) | 1.174 (4) | −0.1115 (8) | 0.053 (8) | 0.60 (2) |
H43A | 0.2542 | 1.14 | −0.1138 | 0.079* | 0.60 (2) |
H43B | 0.2158 | 1.2833 | −0.1061 | 0.079* | 0.60 (2) |
H43C | 0.1925 | 1.1553 | −0.1338 | 0.079* | 0.60 (2) |
N4B | 0.195 (5) | 1.002 (17) | −0.0226 (19) | 0.041 (11) | 0.40 (2) |
H4BA | 0.1672 | 1.0606 | −0.0146 | 0.062* | 0.40 (2) |
H4BB | 0.2281 | 1.0253 | −0.0103 | 0.062* | 0.40 (2) |
H4BC | 0.1867 | 0.9016 | −0.0194 | 0.062* | 0.40 (2) |
C41B | 0.198 (2) | 1.032 (4) | −0.0597 (13) | 0.051 (6) | 0.40 (2) |
H41C | 0.1592 | 1.022 | −0.0718 | 0.061* | 0.40 (2) |
H41D | 0.2204 | 0.9499 | −0.0691 | 0.061* | 0.40 (2) |
C42B | 0.221 (2) | 1.180 (4) | −0.0701 (11) | 0.051 (6) | 0.40 (2) |
H42C | 0.258 | 1.1902 | −0.0568 | 0.061* | 0.40 (2) |
H42D | 0.1967 | 1.2602 | −0.0609 | 0.061* | 0.40 (2) |
C43B | 0.227 (3) | 1.223 (7) | −0.1072 (10) | 0.053 (11) | 0.40 (2) |
H43D | 0.2674 | 1.2206 | −0.1109 | 0.079* | 0.40 (2) |
H43E | 0.2126 | 1.3255 | −0.112 | 0.079* | 0.40 (2) |
H43F | 0.2071 | 1.1496 | −0.1233 | 0.079* | 0.40 (2) |
N5A | 0.131 (3) | 1.012 (8) | 0.2474 (12) | 0.030 (9) | 0.428 (19) |
H5AA | 0.1619 | 1.0355 | 0.2368 | 0.044* | 0.428 (19) |
H5AB | 0.0997 | 1.0327 | 0.2322 | 0.044* | 0.428 (19) |
H5AC | 0.131 | 0.9117 | 0.2533 | 0.044* | 0.428 (19) |
C51A | 0.1291 (19) | 1.108 (4) | 0.2806 (9) | 0.042 (6) | 0.428 (19) |
H51A | 0.0994 | 1.1868 | 0.2762 | 0.051* | 0.428 (19) |
H51B | 0.1653 | 1.1626 | 0.2852 | 0.051* | 0.428 (19) |
C52A | 0.118 (2) | 1.017 (4) | 0.3138 (9) | 0.046 (6) | 0.428 (19) |
H52A | 0.1488 | 0.9429 | 0.3197 | 0.055* | 0.428 (19) |
H52B | 0.0824 | 0.961 | 0.3098 | 0.055* | 0.428 (19) |
C53A | 0.116 (3) | 1.133 (6) | 0.3441 (13) | 0.042 (6) | 0.428 (19) |
H53A | 0.1532 | 1.1753 | 0.3505 | 0.062* | 0.428 (19) |
H53B | 0.1027 | 1.0814 | 0.3646 | 0.062* | 0.428 (19) |
H53C | 0.0899 | 1.2156 | 0.3364 | 0.062* | 0.428 (19) |
N5B | 0.1421 (18) | 1.017 (6) | 0.2545 (8) | 0.027 (7) | 0.572 (19) |
H5BA | 0.1367 | 1.1036 | 0.2413 | 0.04* | 0.572 (19) |
H5BB | 0.1327 | 0.9342 | 0.2407 | 0.04* | 0.572 (19) |
H5BC | 0.1788 | 1.0104 | 0.2632 | 0.04* | 0.572 (19) |
C51B | 0.1057 (13) | 1.022 (3) | 0.2850 (8) | 0.041 (5) | 0.572 (19) |
H51C | 0.1019 | 0.9176 | 0.2946 | 0.049* | 0.572 (19) |
H51D | 0.0678 | 1.0589 | 0.2763 | 0.049* | 0.572 (19) |
C52B | 0.1316 (13) | 1.128 (3) | 0.3143 (6) | 0.046 (5) | 0.572 (19) |
H52C | 0.1253 | 1.2362 | 0.3074 | 0.055* | 0.572 (19) |
H52D | 0.1724 | 1.11 | 0.3187 | 0.055* | 0.572 (19) |
C53B | 0.1030 (19) | 1.092 (5) | 0.3478 (9) | 0.042 (6) | 0.572 (19) |
H53D | 0.102 | 1.1851 | 0.3622 | 0.062* | 0.572 (19) |
H53E | 0.1241 | 1.0127 | 0.3615 | 0.062* | 0.572 (19) |
H53F | 0.0646 | 1.057 | 0.3411 | 0.062* | 0.572 (19) |
N6A | 0.357 (2) | 0.544 (7) | −0.0025 (11) | 0.040 (9) | 0.54 (2) |
H6AA | 0.3792 | 0.4932 | 0.0144 | 0.061* | 0.54 (2) |
H6AB | 0.3224 | 0.499 | −0.0052 | 0.061* | 0.54 (2) |
H6AC | 0.3533 | 0.6429 | 0.0041 | 0.061* | 0.54 (2) |
C61A | 0.3824 (16) | 0.538 (3) | −0.0368 (10) | 0.048 (6) | 0.54 (2) |
H61A | 0.3677 | 0.6216 | −0.0525 | 0.058* | 0.54 (2) |
H61B | 0.4236 | 0.5479 | −0.0326 | 0.058* | 0.54 (2) |
C62A | 0.3674 (16) | 0.389 (3) | −0.0531 (8) | 0.054 (6) | 0.54 (2) |
H62A | 0.3286 | 0.3657 | −0.048 | 0.065* | 0.54 (2) |
H62B | 0.3919 | 0.3113 | −0.0404 | 0.065* | 0.54 (2) |
C63A | 0.370 (2) | 0.364 (5) | −0.0912 (9) | 0.064 (10) | 0.54 (2) |
H63A | 0.3665 | 0.4628 | −0.1035 | 0.095* | 0.54 (2) |
H63B | 0.3394 | 0.297 | −0.1004 | 0.095* | 0.54 (2) |
H63C | 0.406 | 0.3173 | −0.095 | 0.095* | 0.54 (2) |
N6B | 0.369 (3) | 0.554 (9) | 0.0024 (14) | 0.043 (10) | 0.46 (2) |
H6BA | 0.3519 | 0.6429 | −0.0045 | 0.065* | 0.46 (2) |
H6BB | 0.4065 | 0.5725 | 0.0086 | 0.065* | 0.46 (2) |
H6BC | 0.3537 | 0.515 | 0.0213 | 0.065* | 0.46 (2) |
C61B | 0.3632 (18) | 0.442 (4) | −0.0274 (10) | 0.049 (6) | 0.46 (2) |
H61C | 0.3837 | 0.3472 | −0.0201 | 0.059* | 0.46 (2) |
H61D | 0.3231 | 0.4158 | −0.0327 | 0.059* | 0.46 (2) |
C62B | 0.385 (2) | 0.502 (4) | −0.0597 (9) | 0.053 (6) | 0.46 (2) |
H62C | 0.3615 | 0.5928 | −0.0664 | 0.064* | 0.46 (2) |
H62D | 0.4227 | 0.5405 | −0.052 | 0.064* | 0.46 (2) |
C63B | 0.390 (2) | 0.419 (6) | −0.0929 (11) | 0.060 (10) | 0.46 (2) |
H63D | 0.3809 | 0.3108 | −0.0897 | 0.09* | 0.46 (2) |
H63E | 0.4281 | 0.4286 | −0.0994 | 0.09* | 0.46 (2) |
H63F | 0.3635 | 0.4624 | −0.1117 | 0.09* | 0.46 (2) |
N7 | −0.0026 (6) | 0.4752 (14) | 0.0568 (4) | 0.045 (4) | |
H7A | −0.0137 | 0.5628 | 0.0452 | 0.067* | |
H7B | −0.0045 | 0.3961 | 0.0411 | 0.067* | |
H7C | 0.0333 | 0.4859 | 0.0667 | 0.067* | |
C71 | −0.0403 (9) | 0.4433 (18) | 0.0853 (5) | 0.056 (5) | |
H71A | −0.0772 | 0.4071 | 0.0745 | 0.068* | |
H71B | −0.0236 | 0.3626 | 0.1013 | 0.068* | |
C72 | −0.0473 (9) | 0.585 (2) | 0.1055 (5) | 0.064 (5) | |
H72A | −0.0106 | 0.6174 | 0.1175 | 0.077* | |
H72B | −0.0612 | 0.6679 | 0.0891 | 0.077* | |
C73 | −0.0873 (12) | 0.561 (3) | 0.1322 (7) | 0.101 (8) | |
H73A | −0.1234 | 0.5278 | 0.1203 | 0.151* | |
H73B | −0.0922 | 0.6562 | 0.1449 | 0.151* | |
H73C | −0.0727 | 0.4817 | 0.1489 | 0.151* | |
N8 | 0.2967 (7) | 0.5414 (14) | 0.2697 (4) | 0.048 (4) | |
H8A | 0.2697 | 0.4814 | 0.2582 | 0.071* | |
H8B | 0.3305 | 0.5186 | 0.2621 | 0.071* | |
H8C | 0.2884 | 0.6414 | 0.2651 | 0.071* | |
C81 | 0.2988 (14) | 0.513 (3) | 0.3089 (5) | 0.112 (8) | |
H81A | 0.3383 | 0.5187 | 0.3194 | 0.134* | |
H81B | 0.2778 | 0.595 | 0.3198 | 0.134* | |
C82 | 0.2755 (13) | 0.364 (3) | 0.3177 (5) | 0.111 (8) | |
H82A | 0.2993 | 0.2827 | 0.3092 | 0.133* | |
H82B | 0.2377 | 0.3541 | 0.3048 | 0.133* | |
C83 | 0.2709 (10) | 0.341 (2) | 0.3561 (5) | 0.076 (6) | |
H83A | 0.3076 | 0.3566 | 0.3694 | 0.114* | |
H83B | 0.2581 | 0.2363 | 0.3601 | 0.114* | |
H83C | 0.2439 | 0.4136 | 0.3643 | 0.114* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.0200 (3) | 0.0212 (3) | 0.0224 (3) | 0.0004 (2) | 0.0058 (3) | −0.0010 (2) |
Pb2 | 0.0193 (4) | 0.0224 (3) | 0.0251 (3) | 0.0001 (2) | 0.0022 (3) | −0.0013 (2) |
Pb3 | 0.0200 (3) | 0.0208 (3) | 0.0230 (3) | 0.0001 (2) | 0.0054 (3) | −0.0003 (2) |
Pb4 | 0.0196 (4) | 0.0252 (3) | 0.0240 (3) | −0.0013 (2) | 0.0018 (3) | −0.0030 (2) |
Pb5 | 0.0263 (5) | 0.0229 (4) | 0.0328 (5) | 0 | 0.0147 (4) | 0 |
Pb6 | 0.0262 (5) | 0.0230 (4) | 0.0348 (5) | 0.0017 (3) | 0.0140 (4) | 0.0025 (3) |
I1 | 0.0245 (6) | 0.0246 (5) | 0.0328 (6) | 0.0049 (4) | 0.0034 (5) | 0.0004 (4) |
I2 | 0.0290 (6) | 0.0247 (5) | 0.0351 (6) | 0.0048 (4) | 0.0060 (5) | 0.0049 (4) |
I3 | 0.0270 (6) | 0.0246 (5) | 0.0465 (7) | −0.0065 (4) | 0.0112 (5) | −0.0087 (4) |
I4 | 0.0446 (8) | 0.0479 (6) | 0.0224 (6) | 0.0058 (5) | 0.0039 (5) | −0.0004 (4) |
I5 | 0.0329 (7) | 0.0304 (5) | 0.0335 (6) | −0.0141 (4) | 0.0044 (5) | −0.0044 (4) |
I6 | 0.0375 (7) | 0.0549 (7) | 0.0270 (6) | 0.0043 (5) | 0.0106 (5) | −0.0021 (4) |
I7 | 0.0217 (6) | 0.0235 (5) | 0.0437 (6) | 0.0020 (4) | 0.0044 (5) | 0.0005 (4) |
I8 | 0.0276 (6) | 0.0246 (5) | 0.0427 (6) | −0.0029 (4) | −0.0037 (5) | −0.0016 (4) |
I9 | 0.0376 (8) | 0.0671 (7) | 0.0195 (6) | −0.0093 (5) | 0.0030 (5) | −0.0017 (5) |
I10 | 0.0304 (7) | 0.0289 (5) | 0.0449 (7) | 0.0086 (4) | 0.0067 (5) | 0.0130 (4) |
I11 | 0.0461 (8) | 0.0443 (6) | 0.0240 (6) | 0.0021 (5) | 0.0054 (5) | −0.0001 (4) |
I12 | 0.0269 (6) | 0.0227 (5) | 0.0434 (6) | −0.0049 (4) | 0.0104 (5) | −0.0053 (4) |
I13 | 0.0249 (6) | 0.0253 (5) | 0.0316 (6) | 0.0050 (4) | 0.0024 (5) | 0.0004 (4) |
I14 | 0.0308 (6) | 0.0287 (5) | 0.0325 (6) | −0.0126 (4) | 0.0049 (5) | −0.0034 (4) |
I15 | 0.0408 (7) | 0.0562 (6) | 0.0281 (6) | −0.0008 (5) | 0.0130 (5) | −0.0068 (5) |
I16 | 0.0244 (6) | 0.0272 (5) | 0.0431 (6) | 0.0028 (4) | 0.0012 (5) | −0.0043 (4) |
I17 | 0.0249 (6) | 0.0250 (5) | 0.0399 (6) | −0.0020 (4) | −0.0001 (5) | −0.0066 (4) |
I18 | 0.0350 (8) | 0.0652 (7) | 0.0201 (6) | −0.0095 (5) | 0.0028 (5) | −0.0025 (4) |
N1 | 0.066 (8) | 0.042 (8) | 0.028 (8) | 0.002 (7) | 0.017 (7) | −0.002 (6) |
C11 | 0.064 (9) | 0.059 (9) | 0.039 (10) | 0.019 (8) | 0.011 (6) | −0.014 (7) |
C12 | 0.066 (9) | 0.081 (11) | 0.038 (11) | 0.003 (9) | 0.013 (7) | 0.007 (8) |
C13 | 0.063 (9) | 0.068 (12) | 0.083 (17) | 0.005 (11) | 0.004 (10) | 0.008 (11) |
N2 | 0.062 (8) | 0.050 (8) | 0.035 (9) | −0.013 (7) | 0.016 (7) | −0.016 (6) |
C21 | 0.051 (9) | 0.063 (10) | 0.056 (11) | 0.012 (8) | 0.014 (6) | −0.007 (8) |
C22 | 0.062 (9) | 0.066 (10) | 0.049 (11) | 0.000 (9) | 0.018 (7) | −0.007 (8) |
C23 | 0.050 (9) | 0.098 (15) | 0.096 (19) | 0.021 (12) | 0.014 (10) | −0.003 (13) |
N3 | 0.049 (11) | 0.040 (7) | 0.031 (8) | 0.008 (6) | −0.005 (6) | −0.011 (5) |
C31 | 0.042 (11) | 0.076 (10) | 0.036 (10) | 0.009 (8) | −0.004 (7) | −0.009 (7) |
C32 | 0.052 (12) | 0.091 (11) | 0.040 (10) | 0.017 (9) | 0.004 (8) | −0.014 (7) |
C33 | 0.040 (13) | 0.147 (18) | 0.042 (12) | 0.017 (12) | 0.002 (8) | −0.011 (11) |
N4A | 0.02 (2) | 0.030 (12) | 0.044 (10) | 0.003 (14) | −0.002 (13) | 0.004 (10) |
C41A | 0.050 (14) | 0.036 (11) | 0.038 (9) | −0.005 (9) | 0.001 (9) | 0.002 (7) |
C42A | 0.062 (14) | 0.053 (12) | 0.043 (9) | −0.014 (10) | −0.007 (10) | 0.006 (9) |
C43A | 0.07 (2) | 0.05 (2) | 0.034 (11) | −0.017 (15) | 0.004 (14) | −0.009 (12) |
N4B | 0.04 (3) | 0.032 (17) | 0.046 (12) | −0.008 (19) | −0.008 (18) | 0.002 (14) |
C41B | 0.056 (15) | 0.048 (12) | 0.044 (10) | −0.007 (11) | −0.011 (12) | 0.000 (10) |
C42B | 0.058 (15) | 0.056 (12) | 0.038 (11) | −0.009 (11) | −0.006 (12) | 0.007 (10) |
C43B | 0.07 (3) | 0.06 (3) | 0.026 (14) | −0.03 (2) | −0.010 (19) | −0.013 (16) |
N5A | 0.01 (2) | 0.039 (15) | 0.033 (12) | 0.015 (16) | −0.006 (16) | 0.003 (12) |
C51A | 0.034 (13) | 0.059 (13) | 0.032 (9) | −0.002 (11) | −0.006 (11) | −0.004 (9) |
C52A | 0.036 (13) | 0.063 (13) | 0.040 (10) | −0.011 (11) | 0.009 (11) | −0.007 (9) |
C53A | 0.022 (16) | 0.063 (16) | 0.041 (8) | 0.002 (11) | 0.012 (9) | −0.007 (10) |
N5B | 0.011 (17) | 0.042 (12) | 0.026 (12) | −0.011 (12) | −0.003 (12) | 0.010 (11) |
C51B | 0.031 (12) | 0.056 (12) | 0.037 (9) | −0.010 (10) | 0.012 (9) | −0.001 (9) |
C52B | 0.040 (12) | 0.062 (12) | 0.038 (10) | −0.007 (10) | 0.010 (9) | −0.004 (9) |
C53B | 0.022 (16) | 0.063 (16) | 0.041 (8) | 0.002 (11) | 0.012 (9) | −0.007 (10) |
N6A | 0.04 (2) | 0.029 (13) | 0.055 (15) | −0.017 (15) | 0.005 (15) | 0.009 (11) |
C61A | 0.042 (13) | 0.046 (11) | 0.058 (12) | −0.013 (10) | 0.009 (12) | 0.005 (9) |
C62A | 0.048 (14) | 0.050 (11) | 0.063 (12) | 0.001 (11) | −0.001 (13) | −0.004 (9) |
C63A | 0.08 (3) | 0.05 (2) | 0.057 (12) | −0.012 (18) | −0.006 (19) | 0.005 (13) |
N6B | 0.03 (2) | 0.045 (17) | 0.056 (14) | 0.002 (18) | −0.010 (17) | 0.000 (11) |
C61B | 0.039 (14) | 0.042 (12) | 0.063 (12) | −0.014 (11) | −0.005 (12) | −0.002 (9) |
C62B | 0.048 (14) | 0.048 (13) | 0.063 (12) | −0.006 (11) | 0.004 (13) | −0.005 (10) |
C63B | 0.06 (2) | 0.06 (2) | 0.060 (14) | 0.003 (18) | −0.009 (17) | −0.008 (14) |
N7 | 0.044 (11) | 0.046 (8) | 0.042 (9) | 0.005 (6) | −0.006 (6) | −0.010 (6) |
C71 | 0.073 (13) | 0.061 (9) | 0.035 (10) | −0.012 (9) | 0.002 (8) | −0.018 (7) |
C72 | 0.072 (13) | 0.066 (10) | 0.054 (11) | −0.001 (9) | 0.010 (9) | −0.021 (8) |
C73 | 0.09 (2) | 0.14 (2) | 0.072 (17) | 0.018 (15) | 0.033 (13) | −0.018 (13) |
N8 | 0.043 (10) | 0.038 (7) | 0.064 (9) | −0.014 (6) | 0.014 (9) | −0.013 (6) |
C81 | 0.124 (19) | 0.137 (15) | 0.075 (10) | 0.003 (14) | 0.011 (14) | 0.029 (12) |
C82 | 0.128 (19) | 0.137 (15) | 0.070 (11) | 0.013 (14) | 0.026 (14) | 0.038 (11) |
C83 | 0.087 (18) | 0.088 (13) | 0.054 (11) | 0.015 (12) | 0.013 (12) | −0.003 (9) |
Pb1—I1 | 3.2345 (14) | C41B—C42B | 1.482 (19) |
Pb1—I2 | 3.2106 (14) | C41B—H41C | 0.99 |
Pb1—I3 | 3.1546 (14) | C41B—H41D | 0.99 |
Pb1—I4 | 3.1943 (12) | C42B—C43B | 1.482 (19) |
Pb1—I5 | 3.2221 (14) | C42B—H42C | 0.99 |
Pb1—I18 | 3.2197 (13) | C42B—H42D | 0.99 |
Pb2—I1i | 3.4415 (14) | C43B—H43D | 0.98 |
Pb2—I5 | 3.3462 (14) | C43B—H43E | 0.98 |
Pb2—I6 | 3.0753 (12) | C43B—H43F | 0.98 |
Pb2—I7 | 3.0341 (14) | N5A—C51A | 1.52 (3) |
Pb2—I8 | 3.0886 (15) | N5A—H5AA | 0.91 |
Pb2—I9 | 3.3741 (13) | N5A—H5AB | 0.91 |
Pb3—I9 | 3.1977 (13) | N5A—H5AC | 0.91 |
Pb3—I10 | 3.1781 (14) | C51A—C52A | 1.54 (2) |
Pb3—I11 | 3.2098 (13) | C51A—H51A | 0.99 |
Pb3—I12 | 3.1899 (14) | C51A—H51B | 0.99 |
Pb3—I13 | 3.2394 (14) | C52A—C53A | 1.54 (2) |
Pb3—I14 | 3.2225 (14) | C52A—H52A | 0.99 |
Pb4—I13ii | 3.4333 (14) | C52A—H52B | 0.99 |
Pb4—I14 | 3.3796 (13) | C53A—H53A | 0.98 |
Pb4—I15 | 3.0699 (12) | C53A—H53B | 0.98 |
Pb4—I16 | 3.0351 (14) | C53A—H53C | 0.98 |
Pb4—I17 | 3.0788 (15) | N5B—C51B | 1.52 (3) |
Pb4—I18 | 3.3779 (13) | N5B—H5BA | 0.91 |
Pb5—I2 | 3.2154 (13) | N5B—H5BB | 0.91 |
Pb5—I3 | 3.2359 (14) | N5B—H5BC | 0.91 |
Pb5—I4 | 3.2486 (14) | C51B—C52B | 1.535 (19) |
Pb6—I10 | 3.2234 (12) | C51B—H51C | 0.99 |
Pb6—I11 | 3.2397 (14) | C51B—H51D | 0.99 |
Pb6—I12 | 3.2335 (14) | C52B—C53B | 1.536 (19) |
I1—Pb2ii | 3.4415 (14) | C52B—H52C | 0.99 |
I13—Pb4i | 3.4333 (14) | C52B—H52D | 0.99 |
N1—C11 | 1.498 (13) | C53B—H53D | 0.98 |
N1—H1A | 0.91 | C53B—H53E | 0.98 |
N1—H1B | 0.91 | C53B—H53F | 0.98 |
N1—H1C | 0.91 | N6A—C61A | 1.49 (4) |
C11—C12 | 1.439 (18) | N6A—H6AA | 0.91 |
C11—H11A | 0.99 | N6A—H6AB | 0.91 |
C11—H11B | 0.99 | N6A—H6AC | 0.91 |
C12—C13 | 1.445 (19) | C61A—C62A | 1.470 (19) |
C12—H12A | 0.99 | C61A—H61A | 0.99 |
C12—H12B | 0.99 | C61A—H61B | 0.99 |
C13—H13A | 0.98 | C62A—C63A | 1.471 (19) |
C13—H13B | 0.98 | C62A—H62A | 0.99 |
C13—H13C | 0.98 | C62A—H62B | 0.99 |
N2—C21 | 1.500 (13) | C63A—H63A | 0.98 |
N2—H2A | 0.91 | C63A—H63B | 0.98 |
N2—H2B | 0.91 | C63A—H63C | 0.98 |
N2—H2C | 0.91 | N6B—C61B | 1.49 (4) |
C21—C22 | 1.470 (19) | N6B—H6BA | 0.91 |
C21—H21A | 0.99 | N6B—H6BB | 0.91 |
C21—H21B | 0.99 | N6B—H6BC | 0.91 |
C22—C23 | 1.476 (19) | C61B—C62B | 1.471 (19) |
C22—H22A | 0.99 | C61B—H61C | 0.99 |
C22—H22B | 0.99 | C61B—H61D | 0.99 |
C23—H23A | 0.98 | C62B—C63B | 1.471 (19) |
C23—H23B | 0.98 | C62B—H62C | 0.99 |
C23—H23C | 0.98 | C62B—H62D | 0.99 |
N3—C31 | 1.499 (12) | C63B—H63D | 0.98 |
N3—H3A | 0.91 | C63B—H63E | 0.98 |
N3—H3B | 0.91 | C63B—H63F | 0.98 |
N3—H3C | 0.91 | N7—C71 | 1.505 (12) |
C31—C32 | 1.491 (17) | N7—H7A | 0.91 |
C31—H31A | 0.99 | N7—H7B | 0.91 |
C31—H31B | 0.99 | N7—H7C | 0.91 |
C32—C33 | 1.490 (17) | C71—C72 | 1.480 (17) |
C32—H32A | 0.99 | C71—H71A | 0.99 |
C32—H32B | 0.99 | C71—H71B | 0.99 |
C33—H33A | 0.98 | C72—C73 | 1.479 (18) |
C33—H33B | 0.98 | C72—H72A | 0.99 |
C33—H33C | 0.98 | C72—H72B | 0.99 |
N4A—C41A | 1.44 (4) | C73—H73A | 0.98 |
N4A—H4AA | 0.91 | C73—H73B | 0.98 |
N4A—H4AB | 0.91 | C73—H73C | 0.98 |
N4A—H4AC | 0.91 | N8—C81 | 1.506 (13) |
C41A—C42A | 1.479 (19) | N8—H8A | 0.91 |
C41A—H41A | 0.99 | N8—H8B | 0.91 |
C41A—H41B | 0.99 | N8—H8C | 0.91 |
C42A—C43A | 1.482 (19) | C81—C82 | 1.469 (10) |
C42A—H42A | 0.99 | C81—H81A | 0.99 |
C42A—H42B | 0.99 | C81—H81B | 0.99 |
C43A—H43A | 0.98 | C82—C83 | 1.490 (10) |
C43A—H43B | 0.98 | C82—H82A | 0.99 |
C43A—H43C | 0.98 | C82—H82B | 0.99 |
N4B—C41B | 1.44 (4) | C83—H83A | 0.98 |
N4B—H4BA | 0.91 | C83—H83B | 0.98 |
N4B—H4BB | 0.91 | C83—H83C | 0.98 |
N4B—H4BC | 0.91 | ||
I3—Pb1—I4 | 86.58 (3) | C33—C32—H32B | 108.7 |
I3—Pb1—I2 | 88.92 (5) | C31—C32—H32B | 108.7 |
I4—Pb1—I2 | 81.54 (3) | H32A—C32—H32B | 107.6 |
I3—Pb1—I18 | 96.41 (3) | C32—C33—H33A | 109.5 |
I4—Pb1—I18 | 174.93 (4) | C32—C33—H33B | 109.5 |
I2—Pb1—I18 | 102.57 (3) | H33A—C33—H33B | 109.5 |
I3—Pb1—I5 | 174.88 (3) | C32—C33—H33C | 109.5 |
I4—Pb1—I5 | 90.30 (3) | H33A—C33—H33C | 109.5 |
I2—Pb1—I5 | 94.64 (4) | H33B—C33—H33C | 109.5 |
I18—Pb1—I5 | 86.42 (3) | N4A—C41A—C42A | 114 (4) |
I3—Pb1—I1 | 90.17 (4) | N4A—C41A—H41A | 108.7 |
I4—Pb1—I1 | 89.33 (3) | C42A—C41A—H41A | 108.7 |
I2—Pb1—I1 | 170.87 (3) | N4A—C41A—H41B | 108.7 |
I18—Pb1—I1 | 86.56 (3) | C42A—C41A—H41B | 108.7 |
I5—Pb1—I1 | 85.73 (4) | H41A—C41A—H41B | 107.6 |
I7—Pb2—I6 | 88.69 (3) | C41A—C42A—C43A | 116 (3) |
I7—Pb2—I8 | 93.25 (5) | C41A—C42A—H42A | 108.3 |
I6—Pb2—I8 | 99.92 (3) | C43A—C42A—H42A | 108.3 |
I7—Pb2—I5 | 94.80 (4) | C41A—C42A—H42B | 108.3 |
I6—Pb2—I5 | 86.72 (3) | C43A—C42A—H42B | 108.3 |
I8—Pb2—I5 | 169.69 (3) | H42A—C42A—H42B | 107.4 |
I7—Pb2—I9 | 91.63 (3) | C41B—N4B—H4BA | 109.5 |
I6—Pb2—I9 | 171.33 (4) | C41B—N4B—H4BB | 109.5 |
I8—Pb2—I9 | 88.72 (3) | H4BA—N4B—H4BB | 109.5 |
I5—Pb2—I9 | 84.62 (3) | C41B—N4B—H4BC | 109.5 |
I7—Pb2—I1i | 175.05 (3) | H4BA—N4B—H4BC | 109.5 |
I6—Pb2—I1i | 94.06 (3) | H4BB—N4B—H4BC | 109.5 |
I8—Pb2—I1i | 90.34 (4) | N4B—C41B—C42B | 118 (7) |
I5—Pb2—I1i | 81.27 (4) | N4B—C41B—H41C | 107.7 |
I9—Pb2—I1i | 85.03 (3) | C42B—C41B—H41C | 107.7 |
I10—Pb3—I12 | 88.10 (5) | N4B—C41B—H41D | 107.7 |
I10—Pb3—I9 | 99.00 (3) | C42B—C41B—H41D | 107.7 |
I12—Pb3—I9 | 98.88 (3) | H41C—C41B—H41D | 107.1 |
I10—Pb3—I11 | 82.06 (3) | C41B—C42B—C43B | 124 (4) |
I12—Pb3—I11 | 86.82 (3) | C41B—C42B—H42C | 106.4 |
I9—Pb3—I11 | 174.22 (4) | C43B—C42B—H42C | 106.4 |
I10—Pb3—I14 | 95.48 (4) | C41B—C42B—H42D | 106.4 |
I12—Pb3—I14 | 172.79 (3) | C43B—C42B—H42D | 106.4 |
I9—Pb3—I14 | 86.76 (3) | H42C—C42B—H42D | 106.5 |
I11—Pb3—I14 | 87.48 (3) | C42B—C43B—H43D | 109.5 |
I10—Pb3—I13 | 173.25 (3) | C42B—C43B—H43E | 109.5 |
I12—Pb3—I13 | 90.42 (4) | H43D—C43B—H43E | 109.5 |
I9—Pb3—I13 | 87.73 (3) | C42B—C43B—H43F | 109.5 |
I11—Pb3—I13 | 91.28 (3) | H43D—C43B—H43F | 109.5 |
I14—Pb3—I13 | 85.30 (4) | H43E—C43B—H43F | 109.5 |
I16—Pb4—I15 | 90.07 (4) | N5A—C51A—C52A | 114 (4) |
I16—Pb4—I17 | 93.62 (5) | N5A—C51A—H51A | 108.6 |
I15—Pb4—I17 | 98.28 (3) | C52A—C51A—H51A | 108.6 |
I16—Pb4—I18 | 91.48 (3) | N5A—C51A—H51B | 108.6 |
I15—Pb4—I18 | 172.51 (4) | C52A—C51A—H51B | 108.6 |
I17—Pb4—I18 | 88.94 (3) | H51A—C51A—H51B | 107.6 |
I16—Pb4—I14 | 96.72 (4) | C51A—C52A—C53A | 107 (3) |
I15—Pb4—I14 | 87.89 (3) | C51A—C52A—H52A | 110.3 |
I17—Pb4—I14 | 167.96 (3) | C53A—C52A—H52A | 110.3 |
I18—Pb4—I14 | 84.65 (3) | C51A—C52A—H52B | 110.3 |
I16—Pb4—I13ii | 175.71 (3) | C53A—C52A—H52B | 110.3 |
I15—Pb4—I13ii | 93.57 (3) | H52A—C52A—H52B | 108.5 |
I17—Pb4—I13ii | 88.10 (4) | C51B—N5B—H5BA | 109.5 |
I18—Pb4—I13ii | 84.62 (3) | C51B—N5B—H5BB | 109.5 |
I14—Pb4—I13ii | 81.17 (4) | H5BA—N5B—H5BB | 109.5 |
I2iii—Pb5—I2 | 96.26 (5) | C51B—N5B—H5BC | 109.5 |
I2iii—Pb5—I3iii | 87.43 (4) | H5BA—N5B—H5BC | 109.5 |
I2—Pb5—I3iii | 175.76 (3) | H5BB—N5B—H5BC | 109.5 |
I2iii—Pb5—I3 | 175.76 (3) | N5B—C51B—C52B | 110 (3) |
I2—Pb5—I3 | 87.43 (4) | N5B—C51B—H51C | 109.6 |
I3iii—Pb5—I3 | 88.95 (5) | C52B—C51B—H51C | 109.6 |
I2iii—Pb5—I4iii | 80.64 (3) | N5B—C51B—H51D | 109.6 |
I2—Pb5—I4iii | 94.19 (3) | C52B—C51B—H51D | 109.6 |
I3iii—Pb5—I4iii | 84.34 (3) | H51C—C51B—H51D | 108.1 |
I3—Pb5—I4iii | 101.21 (3) | C51B—C52B—C53B | 107 (3) |
I2iii—Pb5—I4 | 94.19 (3) | C51B—C52B—H52C | 110.3 |
I2—Pb5—I4 | 80.64 (3) | C53B—C52B—H52C | 110.3 |
I3iii—Pb5—I4 | 101.21 (3) | C51B—C52B—H52D | 110.3 |
I3—Pb5—I4 | 84.34 (3) | C53B—C52B—H52D | 110.3 |
I4iii—Pb5—I4 | 172.30 (4) | H52C—C52B—H52D | 108.5 |
I10—Pb6—I10iv | 180.00 (3) | C52B—C53B—H53D | 109.5 |
I10—Pb6—I12 | 86.59 (4) | C52B—C53B—H53E | 109.5 |
I10iv—Pb6—I12 | 93.41 (4) | H53D—C53B—H53E | 109.5 |
I10—Pb6—I12iv | 93.41 (4) | C52B—C53B—H53F | 109.5 |
I10iv—Pb6—I12iv | 86.59 (4) | H53D—C53B—H53F | 109.5 |
I12—Pb6—I12iv | 180.00 (3) | H53E—C53B—H53F | 109.5 |
I10—Pb6—I11 | 80.90 (3) | C62A—C61A—N6A | 107 (3) |
I10iv—Pb6—I11 | 99.10 (3) | C62A—C61A—H61A | 110.3 |
I12—Pb6—I11 | 85.59 (3) | N6A—C61A—H61A | 110.3 |
I12iv—Pb6—I11 | 94.41 (3) | C62A—C61A—H61B | 110.3 |
I10—Pb6—I11iv | 99.10 (3) | N6A—C61A—H61B | 110.3 |
I10iv—Pb6—I11iv | 80.90 (3) | H61A—C61A—H61B | 108.5 |
I12—Pb6—I11iv | 94.41 (3) | C61A—C62A—C63A | 121 (3) |
I12iv—Pb6—I11iv | 85.59 (3) | C61A—C62A—H62A | 107.2 |
I11—Pb6—I11iv | 180 | C63A—C62A—H62A | 107.2 |
Pb1—I1—Pb2ii | 171.24 (4) | C61A—C62A—H62B | 107.2 |
Pb1—I2—Pb5 | 77.36 (3) | C63A—C62A—H62B | 107.2 |
Pb1—I3—Pb5 | 77.86 (4) | H62A—C62A—H62B | 106.8 |
Pb1—I4—Pb5 | 77.12 (3) | C61B—N6B—H6BA | 109.5 |
Pb1—I5—Pb2 | 153.08 (4) | C61B—N6B—H6BB | 109.5 |
Pb3—I9—Pb2 | 162.51 (4) | H6BA—N6B—H6BB | 109.5 |
Pb3—I10—Pb6 | 77.69 (3) | C61B—N6B—H6BC | 109.5 |
Pb3—I11—Pb6 | 77.00 (3) | H6BA—N6B—H6BC | 109.5 |
Pb3—I12—Pb6 | 77.37 (4) | H6BB—N6B—H6BC | 109.5 |
Pb3—I13—Pb4i | 171.91 (4) | C62B—C61B—N6B | 112 (4) |
Pb3—I14—Pb4 | 154.23 (4) | C62B—C61B—H61C | 109.1 |
Pb1—I18—Pb4 | 162.42 (4) | N6B—C61B—H61C | 109.1 |
C11—N1—H1A | 109.5 | C62B—C61B—H61D | 109.1 |
C11—N1—H1B | 109.5 | N6B—C61B—H61D | 109.1 |
H1A—N1—H1B | 109.5 | H61C—C61B—H61D | 107.9 |
C11—N1—H1C | 109.5 | C63B—C62B—C61B | 127 (4) |
H1A—N1—H1C | 109.5 | C63B—C62B—H62C | 105.5 |
H1B—N1—H1C | 109.5 | C61B—C62B—H62C | 105.5 |
C12—C11—N1 | 112.3 (16) | C63B—C62B—H62D | 105.5 |
C12—C11—H11A | 109.2 | C61B—C62B—H62D | 105.5 |
N1—C11—H11A | 109.2 | H62C—C62B—H62D | 106.1 |
C12—C11—H11B | 109.2 | C62B—C63B—H63D | 109.5 |
N1—C11—H11B | 109.2 | C62B—C63B—H63E | 109.5 |
H11A—C11—H11B | 107.9 | H63D—C63B—H63E | 109.5 |
C11—C12—C13 | 111.6 (19) | C62B—C63B—H63F | 109.5 |
C11—C12—H12A | 109.3 | H63D—C63B—H63F | 109.5 |
C13—C12—H12A | 109.3 | H63E—C63B—H63F | 109.5 |
C11—C12—H12B | 109.3 | C71—N7—H7A | 109.5 |
C13—C12—H12B | 109.3 | C71—N7—H7B | 109.5 |
H12A—C12—H12B | 108 | H7A—N7—H7B | 109.5 |
C12—C13—H13A | 109.5 | C71—N7—H7C | 109.5 |
C12—C13—H13B | 109.5 | H7A—N7—H7C | 109.5 |
H13A—C13—H13B | 109.5 | H7B—N7—H7C | 109.5 |
C12—C13—H13C | 109.5 | C72—C71—N7 | 109.0 (14) |
H13A—C13—H13C | 109.5 | C72—C71—H71A | 109.9 |
H13B—C13—H13C | 109.5 | N7—C71—H71A | 109.9 |
C21—N2—H2A | 109.5 | C72—C71—H71B | 109.9 |
C21—N2—H2B | 109.5 | N7—C71—H71B | 109.9 |
H2A—N2—H2B | 109.5 | H71A—C71—H71B | 108.3 |
C21—N2—H2C | 109.5 | C73—C72—C71 | 110.4 (17) |
H2A—N2—H2C | 109.5 | C73—C72—H72A | 109.6 |
H2B—N2—H2C | 109.5 | C71—C72—H72A | 109.6 |
C22—C21—N2 | 111.5 (17) | C73—C72—H72B | 109.6 |
C22—C21—H21A | 109.3 | C71—C72—H72B | 109.6 |
N2—C21—H21A | 109.3 | H72A—C72—H72B | 108.1 |
C22—C21—H21B | 109.3 | C72—C73—H73A | 109.5 |
N2—C21—H21B | 109.3 | C72—C73—H73B | 109.5 |
H21A—C21—H21B | 108 | H73A—C73—H73B | 109.5 |
C21—C22—C23 | 113.5 (19) | C72—C73—H73C | 109.5 |
C21—C22—H22A | 108.9 | H73A—C73—H73C | 109.5 |
C23—C22—H22A | 108.9 | H73B—C73—H73C | 109.5 |
C21—C22—H22B | 108.9 | C81—N8—H8A | 109.5 |
C23—C22—H22B | 108.9 | C81—N8—H8B | 109.5 |
H22A—C22—H22B | 107.7 | H8A—N8—H8B | 109.5 |
C22—C23—H23A | 109.5 | C81—N8—H8C | 109.5 |
C22—C23—H23B | 109.5 | H8A—N8—H8C | 109.5 |
H23A—C23—H23B | 109.5 | H8B—N8—H8C | 109.5 |
C22—C23—H23C | 109.5 | C82—C81—N8 | 113.2 (16) |
H23A—C23—H23C | 109.5 | C82—C81—H81A | 108.9 |
H23B—C23—H23C | 109.5 | N8—C81—H81A | 108.9 |
C31—N3—H3A | 109.5 | C82—C81—H81B | 108.9 |
C31—N3—H3B | 109.5 | N8—C81—H81B | 108.9 |
H3A—N3—H3B | 109.5 | H81A—C81—H81B | 107.8 |
C31—N3—H3C | 109.5 | C81—C82—C83 | 114.4 (18) |
H3A—N3—H3C | 109.5 | C81—C82—H82A | 108.7 |
H3B—N3—H3C | 109.5 | C83—C82—H82A | 108.7 |
C32—C31—N3 | 112.4 (14) | C81—C82—H82B | 108.7 |
C32—C31—H31A | 109.1 | C83—C82—H82B | 108.7 |
N3—C31—H31A | 109.1 | H82A—C82—H82B | 107.6 |
C32—C31—H31B | 109.1 | C82—C83—H83A | 109.5 |
N3—C31—H31B | 109.1 | C82—C83—H83B | 109.5 |
H31A—C31—H31B | 107.9 | H83A—C83—H83B | 109.5 |
C33—C32—C31 | 114.2 (18) | C82—C83—H83C | 109.5 |
C33—C32—H32A | 108.7 | H83A—C83—H83C | 109.5 |
C31—C32—H32A | 108.7 | H83B—C83—H83C | 109.5 |
I3—Pb1—I2—Pb5 | 39.32 (3) | I11—Pb6—I10—Pb3 | −46.37 (3) |
I4—Pb1—I2—Pb5 | −47.39 (3) | I11iv—Pb6—I10—Pb3 | 133.63 (3) |
I18—Pb1—I2—Pb5 | 135.64 (3) | I10—Pb3—I11—Pb6 | −46.61 (3) |
I5—Pb1—I2—Pb5 | −137.00 (3) | I12—Pb3—I11—Pb6 | 41.92 (3) |
I2iii—Pb5—I2—Pb1 | 139.73 (3) | I14—Pb3—I11—Pb6 | −142.50 (3) |
I3—Pb5—I2—Pb1 | −38.18 (3) | I13—Pb3—I11—Pb6 | 132.26 (3) |
I4iii—Pb5—I2—Pb1 | −139.24 (3) | I10—Pb6—I11—Pb3 | 45.94 (3) |
I4—Pb5—I2—Pb1 | 46.50 (3) | I10iv—Pb6—I11—Pb3 | −134.06 (3) |
I4—Pb1—I3—Pb5 | 42.66 (3) | I12—Pb6—I11—Pb3 | −41.30 (3) |
I2—Pb1—I3—Pb5 | −38.93 (3) | I12iv—Pb6—I11—Pb3 | 138.70 (3) |
I18—Pb1—I3—Pb5 | −141.46 (3) | I10—Pb3—I12—Pb6 | 40.21 (3) |
I1—Pb1—I3—Pb5 | 131.98 (3) | I9—Pb3—I12—Pb6 | 139.03 (3) |
I2—Pb5—I3—Pb1 | 38.90 (3) | I11—Pb3—I12—Pb6 | −41.94 (3) |
I3iii—Pb5—I3—Pb1 | −143.32 (4) | I13—Pb3—I12—Pb6 | −133.21 (3) |
I4iii—Pb5—I3—Pb1 | 132.66 (3) | I10—Pb6—I12—Pb3 | −39.59 (3) |
I4—Pb5—I3—Pb1 | −41.94 (3) | I10iv—Pb6—I12—Pb3 | 140.41 (3) |
I3—Pb1—I4—Pb5 | −42.61 (3) | I11—Pb6—I12—Pb3 | 41.54 (3) |
I2—Pb1—I4—Pb5 | 46.81 (3) | I11iv—Pb6—I12—Pb3 | −138.46 (3) |
I5—Pb1—I4—Pb5 | 141.45 (3) | I10—Pb3—I14—Pb4 | −87.22 (9) |
I1—Pb1—I4—Pb5 | −132.82 (3) | I9—Pb3—I14—Pb4 | 174.03 (8) |
I2iii—Pb5—I4—Pb1 | −142.54 (3) | I11—Pb3—I14—Pb4 | −5.45 (9) |
I2—Pb5—I4—Pb1 | −46.87 (3) | I13—Pb3—I14—Pb4 | 86.05 (8) |
I3iii—Pb5—I4—Pb1 | 129.25 (3) | I16—Pb4—I14—Pb3 | −84.64 (9) |
I3—Pb5—I4—Pb1 | 41.45 (3) | I15—Pb4—I14—Pb3 | 5.19 (9) |
I4—Pb1—I5—Pb2 | 2.18 (8) | I17—Pb4—I14—Pb3 | 126.39 (14) |
I2—Pb1—I5—Pb2 | 83.72 (8) | I18—Pb4—I14—Pb3 | −175.50 (8) |
I18—Pb1—I5—Pb2 | −173.94 (8) | I13ii—Pb4—I14—Pb3 | 99.13 (8) |
I1—Pb1—I5—Pb2 | −87.12 (8) | I3—Pb1—I18—Pb4 | 178.73 (14) |
I7—Pb2—I5—Pb1 | 84.36 (8) | I2—Pb1—I18—Pb4 | 88.40 (15) |
I6—Pb2—I5—Pb1 | −4.05 (8) | I5—Pb1—I18—Pb4 | −5.55 (15) |
I8—Pb2—I5—Pb1 | −134.45 (16) | I1—Pb1—I18—Pb4 | −91.49 (15) |
I9—Pb2—I5—Pb1 | 175.55 (8) | I16—Pb4—I18—Pb1 | −88.73 (15) |
I1i—Pb2—I5—Pb1 | −98.66 (8) | I17—Pb4—I18—Pb1 | 177.68 (15) |
I10—Pb3—I9—Pb2 | −92.89 (15) | I14—Pb4—I18—Pb1 | 7.89 (15) |
I12—Pb3—I9—Pb2 | 177.64 (14) | I13ii—Pb4—I18—Pb1 | 89.49 (15) |
I14—Pb3—I9—Pb2 | 2.15 (15) | N1—C11—C12—C13 | 173.7 (15) |
I13—Pb3—I9—Pb2 | 87.57 (15) | N2—C21—C22—C23 | −176.6 (16) |
I7—Pb2—I9—Pb3 | 90.08 (15) | N3—C31—C32—C33 | −179.3 (17) |
I8—Pb2—I9—Pb3 | −176.70 (15) | N4A—C41A—C42A—C43A | −168 (5) |
I5—Pb2—I9—Pb3 | −4.59 (15) | N4B—C41B—C42B—C43B | 178 (8) |
I1i—Pb2—I9—Pb3 | −86.26 (15) | N5A—C51A—C52A—C53A | −178 (4) |
I12—Pb3—I10—Pb6 | −40.30 (3) | N5B—C51B—C52B—C53B | −164 (3) |
I9—Pb3—I10—Pb6 | −138.99 (3) | N6A—C61A—C62A—C63A | 160 (5) |
I11—Pb3—I10—Pb6 | 46.75 (3) | N6B—C61B—C62B—C63B | 174 (6) |
I14—Pb3—I10—Pb6 | 133.43 (3) | N7—C71—C72—C73 | 176 (2) |
I12—Pb6—I10—Pb3 | 39.71 (3) | N8—C81—C82—C83 | −173 (2) |
I12iv—Pb6—I10—Pb3 | −140.29 (3) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x, y, −z+1/2; (iv) −x+1, −y+2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I1i | 0.91 | 3.20 | 3.795 (13) | 125 |
N1—H1B···I14 | 0.91 | 2.99 | 3.732 (13) | 140 |
N1—H1B···I13 | 0.91 | 3.20 | 3.793 (13) | 125 |
N1—H1C···I5 | 0.91 | 2.80 | 3.701 (13) | 169 |
N2—H2A···I14 | 0.91 | 2.79 | 3.694 (15) | 173 |
N2—H2B···I5 | 0.91 | 3.01 | 3.713 (14) | 135 |
N2—H2B···I1 | 0.91 | 3.14 | 3.768 (15) | 128 |
N2—H2C···I13ii | 0.91 | 3.08 | 3.765 (13) | 133 |
N3—H3A···I8 | 0.91 | 2.74 | 3.631 (14) | 166 |
N3—H3B···I7v | 0.91 | 2.89 | 3.678 (12) | 146 |
N3—H3B···I7 | 0.91 | 3.17 | 3.759 (14) | 125 |
N3—H3C···I9v | 0.91 | 2.76 | 3.623 (16) | 160 |
N4A—H4AA···I15 | 0.91 | 2.78 | 3.68 (10) | 174 |
N4A—H4AB···I17i | 0.91 | 2.97 | 3.70 (8) | 138 |
N4A—H4AB···I16 | 0.91 | 3.16 | 3.80 (5) | 130 |
N4A—H4AC···I13 | 0.91 | 3.02 | 3.77 (8) | 141 |
N4A—H4AC···I14 | 0.91 | 3.23 | 3.88 (4) | 130 |
N4B—H4BA···I17i | 0.91 | 2.67 | 3.56 (14) | 168 |
N4B—H4BB···I13 | 0.91 | 3.24 | 3.94 (13) | 136 |
N4B—H4BC···I15 | 0.91 | 2.93 | 3.66 (16) | 138 |
N4B—H4BC···I16 | 0.91 | 3.01 | 3.61 (9) | 125 |
N5A—H5AA···I1i | 0.91 | 3.04 | 3.83 (7) | 146 |
N5A—H5AB···I3i | 0.91 | 2.94 | 3.69 (7) | 142 |
N5A—H5AB···I2 | 0.91 | 2.93 | 3.52 (6) | 123 |
N5A—H5AC···I4 | 0.91 | 3.05 | 3.96 (7) | 179 |
N5B—H5BA···I1i | 0.91 | 3.16 | 3.79 (4) | 128 |
N5B—H5BA···I3i | 0.91 | 3.22 | 3.95 (5) | 139 |
N5B—H5BB···I2 | 0.91 | 3.10 | 3.85 (4) | 142 |
N5B—H5BC···I6 | 0.91 | 2.70 | 3.60 (4) | 168 |
N6A—H6AA···I12ii | 0.91 | 3.00 | 3.87 (7) | 162 |
N6A—H6AB···I15 | 0.91 | 3.02 | 3.66 (6) | 129 |
N6A—H6AB···I13ii | 0.91 | 3.12 | 3.73 (5) | 126 |
N6A—H6AC···I11 | 0.91 | 3.03 | 3.77 (6) | 140 |
N6A—H6AC···I14 | 0.91 | 3.30 | 3.92 (4) | 127 |
N6B—H6BA···I11 | 0.91 | 2.93 | 3.71 (8) | 146 |
N6B—H6BB···I10 | 0.91 | 2.95 | 3.64 (5) | 134 |
N6B—H6BB···I12ii | 0.91 | 3.26 | 3.67 (8) | 110 |
N6B—H6BC···I13ii | 0.91 | 3.08 | 3.88 (8) | 147 |
N7—H7A···I17vi | 0.91 | 2.81 | 3.631 (15) | 150 |
N7—H7B···I16vi | 0.91 | 2.90 | 3.669 (14) | 144 |
N7—H7B···I17 | 0.91 | 3.14 | 3.754 (13) | 127 |
N7—H7C···I18 | 0.91 | 2.74 | 3.645 (16) | 171 |
N8—H8A···I1 | 0.91 | 2.91 | 3.751 (14) | 154 |
N8—H8B···I8ii | 0.91 | 2.93 | 3.717 (15) | 146 |
N8—H8B···I7 | 0.91 | 3.11 | 3.689 (14) | 123 |
N8—H8C···I6 | 0.91 | 2.90 | 3.679 (12) | 145 |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (v) −x+1, y, −z+1/2; (vi) −x, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | (C3H10N)8[Pb5I18] |
Mr | 3801.11 |
Crystal system, space group | Monoclinic, P2/c |
Temperature (K) | 173 |
a, b, c (Å) | 23.988 (5), 8.754 (5), 37.986 (5) |
β (°) | 95.718 (5) |
V (Å3) | 7937 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 17.60 |
Crystal size (mm) | 0.44 × 0.06 × 0.06 |
Data collection | |
Diffractometer | Bruker SMART-NT CCD area-detector diffractometer |
Absorption correction | Integration (XPREP; Bruker, 1999) |
Tmin, Tmax | 0.076, 0.392 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 52039, 13878, 9140 |
Rint | 0.090 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.108, 1.00 |
No. of reflections | 13878 |
No. of parameters | 625 |
No. of restraints | 470 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.21, −1.85 |
Computer programs: SMART-NT (Bruker, 1998), SAINT-Plus (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999), WinGX (Farrugia, 1999) and PLATON (Spek, 2002).
Pb1—I1 | 3.2345 (14) | Pb3—I12 | 3.1899 (14) |
Pb1—I2 | 3.2106 (14) | Pb3—I13 | 3.2394 (14) |
Pb1—I3 | 3.1546 (14) | Pb3—I14 | 3.2225 (14) |
Pb1—I4 | 3.1943 (12) | Pb4—I13ii | 3.4333 (14) |
Pb1—I5 | 3.2221 (14) | Pb4—I14 | 3.3796 (13) |
Pb1—I18 | 3.2197 (13) | Pb4—I15 | 3.0699 (12) |
Pb2—I1i | 3.4415 (14) | Pb4—I16 | 3.0351 (14) |
Pb2—I5 | 3.3462 (14) | Pb4—I17 | 3.0788 (15) |
Pb2—I6 | 3.0753 (12) | Pb4—I18 | 3.3779 (13) |
Pb2—I7 | 3.0341 (14) | Pb5—I2 | 3.2154 (13) |
Pb2—I8 | 3.0886 (15) | Pb5—I3 | 3.2359 (14) |
Pb2—I9 | 3.3741 (13) | Pb5—I4 | 3.2486 (14) |
Pb3—I9 | 3.1977 (13) | Pb6—I10 | 3.2234 (12) |
Pb3—I10 | 3.1781 (14) | Pb6—I11 | 3.2397 (14) |
Pb3—I11 | 3.2098 (13) | Pb6—I12 | 3.2335 (14) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I1i | 0.91 | 3.20 | 3.795 (13) | 125 |
N1—H1B···I14 | 0.91 | 2.99 | 3.732 (13) | 140 |
N1—H1B···I13 | 0.91 | 3.20 | 3.793 (13) | 125 |
N1—H1C···I5 | 0.91 | 2.80 | 3.701 (13) | 169 |
N2—H2A···I14 | 0.91 | 2.79 | 3.694 (15) | 173 |
N2—H2B···I5 | 0.91 | 3.01 | 3.713 (14) | 135 |
N2—H2B···I1 | 0.91 | 3.14 | 3.768 (15) | 128 |
N2—H2C···I13ii | 0.91 | 3.08 | 3.765 (13) | 133 |
N3—H3A···I8 | 0.91 | 2.74 | 3.631 (14) | 166 |
N3—H3B···I7iii | 0.91 | 2.89 | 3.678 (12) | 146 |
N3—H3B···I7 | 0.91 | 3.17 | 3.759 (14) | 125 |
N3—H3C···I9iii | 0.91 | 2.76 | 3.623 (16) | 160 |
N4A—H4AA···I15 | 0.91 | 2.78 | 3.68 (10) | 174 |
N4A—H4AB···I17i | 0.91 | 2.97 | 3.70 (8) | 138 |
N4A—H4AB···I16 | 0.91 | 3.16 | 3.80 (5) | 130 |
N4A—H4AC···I13 | 0.91 | 3.02 | 3.77 (8) | 141 |
N4A—H4AC···I14 | 0.91 | 3.23 | 3.88 (4) | 130 |
N4B—H4BA···I17i | 0.91 | 2.67 | 3.56 (14) | 168 |
N4B—H4BB···I13 | 0.91 | 3.24 | 3.94 (13) | 136 |
N4B—H4BC···I15 | 0.91 | 2.93 | 3.66 (16) | 138 |
N4B—H4BC···I16 | 0.91 | 3.01 | 3.61 (9) | 125 |
N5A—H5AA···I1i | 0.91 | 3.04 | 3.83 (7) | 146 |
N5A—H5AB···I3i | 0.91 | 2.94 | 3.69 (7) | 142 |
N5A—H5AB···I2 | 0.91 | 2.93 | 3.52 (6) | 123 |
N5A—H5AC···I4 | 0.91 | 3.05 | 3.96 (7) | 179 |
N5B—H5BA···I1i | 0.91 | 3.16 | 3.79 (4) | 128 |
N5B—H5BA···I3i | 0.91 | 3.22 | 3.95 (5) | 139 |
N5B—H5BB···I2 | 0.91 | 3.10 | 3.85 (4) | 142 |
N5B—H5BC···I6 | 0.91 | 2.70 | 3.60 (4) | 168 |
N6A—H6AA···I12ii | 0.91 | 3.00 | 3.87 (7) | 162 |
N6A—H6AB···I15 | 0.91 | 3.02 | 3.66 (6) | 129 |
N6A—H6AB···I13ii | 0.91 | 3.12 | 3.73 (5) | 126 |
N6A—H6AC···I11 | 0.91 | 3.03 | 3.77 (6) | 140 |
N6A—H6AC···I14 | 0.91 | 3.30 | 3.92 (4) | 127 |
N6B—H6BA···I11 | 0.91 | 2.93 | 3.71 (8) | 146 |
N6B—H6BB···I10 | 0.91 | 2.95 | 3.64 (5) | 134 |
N6B—H6BB···I12ii | 0.91 | 3.26 | 3.67 (8) | 110 |
N6B—H6BC···I13ii | 0.91 | 3.08 | 3.88 (8) | 147 |
N7—H7A···I17iv | 0.91 | 2.81 | 3.631 (15) | 150 |
N7—H7B···I16iv | 0.91 | 2.90 | 3.669 (14) | 144 |
N7—H7B···I17 | 0.91 | 3.14 | 3.754 (13) | 127 |
N7—H7C···I18 | 0.91 | 2.74 | 3.645 (16) | 171 |
N8—H8A···I1 | 0.91 | 2.91 | 3.751 (14) | 154 |
N8—H8B···I8ii | 0.91 | 2.93 | 3.717 (15) | 146 |
N8—H8B···I7 | 0.91 | 3.11 | 3.689 (14) | 123 |
N8—H8C···I6 | 0.91 | 2.90 | 3.679 (12) | 145 |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x+1, y, −z+1/2; (iv) −x, −y+1, −z. |
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Compounds belonging to the hybrid system (C3H7NH3)2[MCl4] (M = Cu, Mn, Cd, Pd and Pb) have been extensively investigated for their phase behaviour (Mitzi, 1999; Depmeier, 1981; Doudin & Chapuis, 1990; Meresse & Daoud, 1989; Willett & Willett, 1977). The hybrid perovskites consist of inorganic semiconducting layers of [MX4]2− perovskite sheets and organic ammonium cation (R—NH3)+ bilayers. When trying to synthesize the compound (C3H7NH3)2PbI4, a different inorganic motif was observed. A view of the asymmetric unit is given in Fig. 1. Instead of the expected sheets of purely corner-sharing octahedra, the lead iodide layers can be built up from PbI6 octahedra linked via corners into nominal zigzag chains that are trans to each other along the crystallographic b axis. Adjacent parallel chains are linked via face-shared octahedra to create infinite sheets parallel to the (201) plane through the unit cell.
Fig. 2 clearly displays the two-dimensional arrangement in which layers of 3-propylammonium molecules are embedded between two consecutive inorganic [Pb5I18] sheets, forming an alternated organic inorganic layered structure. In the direction perpendicular to the layers, the crystal cohesion is achieved by N—H···I hydrogen bridges, related to the NH3 polar groups. There are no van der Waals forces between two adjacent molecules. In the direction parallel to the layers, the cohesion is achieved by strong ionic bonds between axial and equatorial I and Pb atoms.
The inorganic layer is built up from corner-sharing and face-sharing PbI6 octahedra (see Fig. 3). The asymmetric unit consists of four Pb atoms on general positions that undergo corner-sharing of cis-related iodides to form a square, similiar to the corner-sharing hybrid perovskites. The sequence is Pb1—I5—Pb2—I9—Pb3—I14—Pb4—I18—Pb1, viz the Pb atoms are at the corners. Two of these corner-shared squares are connected to each other via atoms I1 and I13. This generates another square, where the sequence is now Pb1—I1—Pb2—I9—Pb3—I13—Pb4—I18—Pb1, which is at right angles to the former square because I1 is cis to I5 and I13 is cis to I14. The squares then form a zigzag sequence, running along the b axis. The two Pb atoms that are at opposite ends of the squares, Pb1 and Pb3, connect adjacent zigzag squares via atoms Pb5 and Pb6, respectively, on special positions, by sharing faces. Atoms I2, I3 and I4 make up the face shared between atoms Pb1 and Pb5, and similarly, atoms I10, I11 and I12 are shared by atoms Pb3 and Pb6. The Pb atoms show different degrees of distortion. The central face-sharing atoms Pb5 and Pb6 each have three unique Pb—I bond lengths only by virtue of their special positions on a twofold axis and a centre of inversion, respectively. All six bond lengths are in a narrow range from 3.2154 (13) to 3.2486 (14) Å. The largest range of bond lengths observed for atoms Pb2 and Pb4, which only undergo corner-sharing with three I atoms. The I atoms that are not involved in any sharing with adjacent octahedra, namely I6, I7 and I8 for Pb2, and I15, I16 and I17 for Pb4, have the shortest bond lengths [3.0341 (14) to 3.0886 (15) Å]. In contrast, the bond lengths to the corner-shared iodides are the longest in the structure [3.3462 (14) to 3.4415 (14) Å]. The Pb1 and Pb3 octahedra, which have three I atoms involved in corner-sharing and three I atoms face-sharing, have a narrow range for all six Pb—I bonds [3.1546 (14) Å to 3.2394 (14) Å), regardless of which type of sharing they are involved in.
There are eight crystallographically independent 3-propylammonium cations in the asymmetric unit (cat1 containing atom N1, etc.), which fill the gaps between the lead iodide systems. Cat4, cat5 and cat6 are disordered. The cations are maximally extended with the moduli of the N—C—C—C torsion angles in the 160 (5)–179.3 (17)° range. The cations are held in place above the gaps by hydrogen-bonding interactions with the I atoms. Cat1, cat2 cat3, cat7 and cat8 have two simple N—H···I bonds and a bifurcated bond. The hydrogen bonds of the three disordered cations are also listed in Table 2. The hydrogen–acceptor distances range from 2.74 to 3.30 Å.