Bis(propane-1,2-diammonium) hexa­iodo­plumbate(II) trihydrate

The title compound, [NH₃CH₂CH(NH₃)CH₃]₂[PbI₆]·3H₂O, crystallizes as an organic-inorganic hybrid, consisting of alternating inorganic and organic layers. The ionic layer consists of isolated [PbI₆]^4- octa­hedra. The hydro­carbon layer has one propane-1,2-diammonium cation in the asymmetric unit which links to the ionic layer via hydrogen bonding. Two solvent water mol­ecules lie between the anions and cations. The Pb atom lies on a centre of inversion.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](b-I) = 0.001 Å
• Disorder in main residue
• R factor = 0.030
• wR factor = 0.059
• Data-to-parameter ratio = 27.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.39
PLAT301_ALERT_3_C Main Residue  Disorder .........................      12.00 Perc.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H11    ..  I3      ..       3.31 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          6

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; 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, 2003).

Bis(propane-1,2-diammonium) hexaiodoplumbate(II) dihydrate

Crystal data

(C3H12N2)2[PbI6]·3H2O	F(000) = 2072
Mr = 1174.93	Dx = 3.018 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 865 reflections
a = 15.093 (3) Å	θ = 3.7–28.1°
b = 9.297 (2) Å	µ = 13.69 mm^−1
c = 19.142 (4) Å	T = 173 K
β = 105.664 (4)°	Cubic, colourless
V = 2586.3 (9) Å^3	0.22 × 0.18 × 0.18 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	2629 reflections with I > 2σ(I)
φ and ω scans	Rint = 0.050
Absorption correction: integration (XPREP; Bruker, 1999)	θmax = 28°, θmin = 2.2°
Tmin = 0.105, Tmax = 0.216	h = −18→19
8378 measured reflections	k = −12→9
3119 independent reflections	l = −19→25

Refinement

Refinement on F^2	89 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.030	w = 1/[σ^2(Fo^2) + (0.0027P)^2 + 27.3459P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.059	(Δ/σ)max = 0.001
S = 1.05	Δρmax = 1.23 e Å^−3
3119 reflections	Δρmin = −1.63 e Å^−3
112 parameters

Special details

Experimental. Numerical integration absroption 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.1586 (5)	0.2309 (8)	0.0906 (4)	0.0407 (15)
H1D	0.1965	0.281	0.0632	0.049*	0.420 (11)
H1E	0.1904	0.1417	0.112	0.049*	0.420 (11)
H1F	0.1893	0.2938	0.0625	0.049*	0.580 (11)
H1G	0.1929	0.1389	0.0984	0.049*	0.580 (11)
C3	0.1026 (6)	0.2395 (8)	0.2053 (4)	0.0500 (19)
H3A	0.0904	0.3051	0.2417	0.06*	0.420 (11)
H3B	0.1493	0.1691	0.2293	0.06*	0.420 (11)
H3C	0.0458	0.1894	0.1804	0.06*	0.420 (11)
H3D	0.1138	0.2874	0.2525	0.06*	0.580 (11)
H3E	0.1119	0.1357	0.2127	0.06*	0.580 (11)
H3F	0.0393	0.2581	0.1768	0.06*	0.580 (11)
N1	0.0640 (4)	0.1993 (6)	0.0432 (3)	0.0317 (12)
H1A	0.0327	0.1452	0.0683	0.048*
H1B	0.0684	0.1503	0.0031	0.048*
H1C	0.0333	0.2834	0.0294	0.048*
N2A	0.2252 (8)	0.3907 (13)	0.1921 (6)	0.039 (3)	0.420 (11)
H2AA	0.2127	0.4667	0.2178	0.059*	0.420 (11)
H2AB	0.2592	0.4212	0.1622	0.059*	0.420 (11)
H2AC	0.2575	0.3233	0.2232	0.059*	0.420 (11)
C2A	0.1387 (14)	0.3279 (13)	0.1486 (7)	0.040 (3)	0.420 (11)
H2A	0.094	0.405	0.126	0.048*	0.420 (11)
N2B	0.1530 (6)	0.4527 (9)	0.1525 (5)	0.034 (2)	0.580 (11)
H2BA	0.1966	0.4931	0.1338	0.051*	0.580 (11)
H2BB	0.1546	0.4953	0.1956	0.051*	0.580 (11)
H2BC	0.0965	0.4656	0.121	0.051*	0.580 (11)
C2B	0.1714 (9)	0.2993 (14)	0.1638 (5)	0.041 (3)	0.580 (11)
H2B	0.2361	0.2845	0.1938	0.049*	0.580 (11)
O1	0.5	0.2599 (9)	0.25	0.0476 (18)
H11	0.5049	0.3397	0.2816	0.057*
O2	0.3399 (4)	0.0918 (7)	0.2202 (3)	0.0564 (15)
H21	0.3931	0.1507	0.2337	0.068*
H22	0.3408	0.0513	0.1752	0.068*
I1	0.37619 (3)	0.50482 (4)	0.09914 (2)	0.02928 (10)
I2	0.09735 (3)	0.50927 (5)	−0.06363 (2)	0.03362 (11)
I3	0.14342 (3)	0.82027 (5)	0.11916 (2)	0.03851 (12)
Pb1	0.25	0.75	0	0.02627 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.043 (3)	0.042 (4)	0.033 (3)	−0.018 (3)	0.005 (3)	0.004 (3)
C3	0.074 (5)	0.044 (4)	0.032 (3)	−0.025 (4)	0.013 (3)	0.002 (3)
N1	0.036 (3)	0.030 (3)	0.032 (3)	−0.010 (2)	0.014 (2)	−0.005 (2)
N2A	0.034 (7)	0.039 (8)	0.041 (7)	−0.008 (5)	0.005 (5)	−0.003 (5)
C2A	0.052 (8)	0.037 (7)	0.020 (5)	−0.021 (6)	−0.007 (5)	0.009 (4)
N2B	0.030 (5)	0.037 (4)	0.033 (5)	−0.003 (4)	0.006 (4)	0.007 (3)
C2B	0.055 (7)	0.037 (5)	0.022 (4)	−0.018 (5)	−0.002 (4)	0.014 (4)
O1	0.051 (4)	0.058 (5)	0.039 (4)	0	0.019 (3)	0
O2	0.057 (3)	0.080 (4)	0.036 (3)	−0.008 (3)	0.019 (2)	0.003 (3)
I1	0.0299 (2)	0.0274 (2)	0.0315 (2)	0.00034 (17)	0.00998 (16)	0.00440 (16)
I2	0.0361 (2)	0.0282 (2)	0.0404 (2)	−0.00279 (18)	0.01695 (19)	0.00212 (18)
I3	0.0363 (2)	0.0508 (3)	0.0339 (2)	−0.0034 (2)	0.01882 (19)	−0.0002 (2)
Pb1	0.02340 (15)	0.02966 (17)	0.02823 (16)	0.00130 (14)	0.01120 (12)	0.00321 (14)

Geometric parameters (Å, º)

C1—N1	1.500 (8)	N2A—H2AA	0.91
C1—C2B	1.503 (12)	N2A—H2AB	0.91
C1—C2A	1.521 (13)	N2A—H2AC	0.91
C1—H1D	0.99	C2A—H2A	1
C1—H1E	0.99	N2B—C2B	1.458 (16)
C1—H1F	0.99	N2B—H2BA	0.91
C1—H1G	0.99	N2B—H2BB	0.91
C3—C2B	1.570 (11)	N2B—H2BC	0.91
C3—C2A	1.572 (12)	C2B—H2B	1
C3—H3A	0.98	O1—H11	0.9471
C3—H3B	0.98	O2—H21	0.9484
C3—H3C	0.98	O2—H22	0.9431
C3—H3D	0.98	I1—Pb1	3.2361 (6)
C3—H3E	0.98	I2—Pb1	3.2071 (6)
C3—H3F	0.98	I3—Pb1	3.1935 (6)
N1—H1A	0.91	Pb1—I3^i	3.1935 (6)
N1—H1B	0.91	Pb1—I2^i	3.2071 (6)
N1—H1C	0.91	Pb1—I1^i	3.2361 (6)
N2A—C2A	1.47 (2)
N1—C1—C2B	120.6 (7)	H1A—N1—H1B	109.5
N1—C1—C2A	102.4 (9)	C1—N1—H1C	109.5
N1—C1—H1D	111.3	H1A—N1—H1C	109.5
C2B—C1—H1D	110.3	H1B—N1—H1C	109.5
C2A—C1—H1D	111.3	C2A—N2A—H2AA	109.5
N1—C1—H1E	111.3	C2A—N2A—H2AB	109.5
C2B—C1—H1E	92.4	H2AA—N2A—H2AB	109.5
C2A—C1—H1E	111.3	C2A—N2A—H2AC	109.5
H1D—C1—H1E	109.2	H2AA—N2A—H2AC	109.5
N1—C1—H1F	107.2	H2AB—N2A—H2AC	109.5
C2B—C1—H1F	107.2	N2A—C2A—C1	109.3 (12)
C2A—C1—H1F	105.1	N2A—C2A—C3	103.7 (10)
H1E—C1—H1F	118.3	C1—C2A—C3	111.6 (8)
N1—C1—H1G	107.2	N2A—C2A—H2A	110.7
C2B—C1—H1G	107.2	C1—C2A—H2A	110.7
C2A—C1—H1G	126.9	C3—C2A—H2A	110.7
H1D—C1—H1G	97.7	C2B—N2B—H2BA	109.5
H1F—C1—H1G	106.8	C2B—N2B—H2BB	109.5
C2B—C3—H3A	114.7	H2BA—N2B—H2BB	109.5
C2A—C3—H3A	109.5	C2B—N2B—H2BC	109.5
C2B—C3—H3B	89.1	H2BA—N2B—H2BC	109.5
C2A—C3—H3B	109.5	H2BB—N2B—H2BC	109.5
H3A—C3—H3B	109.5	N2B—C2B—C1	107.7 (9)
C2B—C3—H3C	122.2	N2B—C2B—C3	107.2 (10)
C2A—C3—H3C	109.5	C1—C2B—C3	112.7 (7)
H3A—C3—H3C	109.5	N2B—C2B—H2B	109.7
H3B—C3—H3C	109.5	C1—C2B—H2B	109.7
C2B—C3—H3D	109.5	C3—C2B—H2B	109.7
C2A—C3—H3D	113.2	H21—O2—H22	105.1
H3B—C3—H3D	87.1	I3—Pb1—I3^i	180
H3C—C3—H3D	125.1	I3—Pb1—I2^i	91.988 (16)
C2B—C3—H3E	109.5	I3^i—Pb1—I2^i	88.012 (16)
C2A—C3—H3E	123.4	I3—Pb1—I2	88.013 (16)
H3A—C3—H3E	123.9	I3^i—Pb1—I2	91.987 (16)
H3C—C3—H3E	70.9	I2^i—Pb1—I2	180
H3D—C3—H3E	109.5	I3—Pb1—I1^i	86.823 (17)
C2B—C3—H3F	109.5	I3^i—Pb1—I1^i	93.177 (17)
C2A—C3—H3F	89.4	I2^i—Pb1—I1^i	88.847 (19)
H3A—C3—H3F	86.8	I2—Pb1—I1^i	91.153 (18)
H3B—C3—H3F	148	I3—Pb1—I1	93.177 (17)
H3D—C3—H3F	109.5	I3^i—Pb1—I1	86.823 (17)
H3E—C3—H3F	109.5	I2^i—Pb1—I1	91.153 (19)
C1—N1—H1A	109.5	I2—Pb1—I1	88.847 (18)
C1—N1—H1B	109.5	I1^i—Pb1—I1	180.000 (10)
N1—C1—C2A—N2A	−169.5 (9)	N1—C1—C2B—N2B	−78.4 (9)
C2B—C1—C2A—N2A	41.0 (17)	C2A—C1—C2B—N2B	−43.2 (17)
N1—C1—C2A—C3	76.4 (13)	N1—C1—C2B—C3	39.7 (14)
C2B—C1—C2A—C3	−73.1 (12)	C2A—C1—C2B—C3	74.9 (12)
C2B—C3—C2A—N2A	−45.7 (18)	C2A—C3—C2B—N2B	42.7 (16)
C2B—C3—C2A—C1	71.8 (12)	C2A—C3—C2B—C1	−75.7 (12)

Symmetry code: (i) −x+1/2, −y+3/2, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···I1^ii	0.91	2.9	3.753 (5)	158
N1—H1B···I1^iii	0.91	2.74	3.629 (5)	167
N1—H1C···I2^iv	0.91	2.96	3.733 (6)	144
N2A—H2AA···O2^v	0.91	1.98	2.859 (13)	164
N2A—H2AB···I1	0.91	2.52	3.416 (10)	170
N2A—H2AC···O2	0.91	2.49	3.241 (15)	140
N2A—H2AC···I3^vi	0.91	2.98	3.681 (12)	135
N2B—H2BA···I1	0.91	2.96	3.805 (9)	155
N2B—H2BB···O2^v	0.91	1.83	2.735 (10)	176
N2B—H2BC···I2^iv	0.91	2.84	3.718 (9)	162
O1—H11···I1^vii	0.95	2.93	3.755 (5)	147
O1—H11···I3^vi	0.95	3.31	3.7684 (14)	112
O2—H21···O1	0.95	1.86	2.803 (7)	173
O2—H22···I2^iii	0.94	2.61	3.506 (5)	158

Symmetry codes: (ii) x−1/2, y−1/2, z; (iii) −x+1/2, −y+1/2, −z; (iv) −x, −y+1, −z; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1, y, −z+1/2.