catena-Poly[heptyl-enedi-ammonium [[tetra-chloridobismuthate(III)]-μ-chlorido]].

The title organic-inorganic hybrid compound, {(C7H20N2)[BiCl5]} n , consists of distorted corner-joined [BiCl6] octa-hedra forming zigzag polymeric anionic chains parallel to [001], separated by columns of heptyl-enedi-ammonium cations. The asymmetric unit contains two crystallographically independent bis-muth metal atoms, one of which lies on an inversion centre and the other on a twofold axis. In the crystal, the polymeric chains and cations are linked by N-H⋯Cl hydrogen bonds, forming undulating layers parallel to (110).

Related literature

For potential applications of alkyl­ammonium halogenido­antim­onates and -bismuthates, see: Ciapala et al. (1997 ▶); Bednarska-Bolek et al. (2000 ▶); Bator et al. (1998 ▶). For the structures of related compounds see: Ouasri et al. (2001 ▶, 2012 ▶); Jeghnou et al. (2005 ▶); Rhandour et al. (2011 ▶).

Experimental

Crystal data

(C7H20N2)[BiCl5]

M = 518.48

Orthorhombic,

a = 12.2451 (5) Å

b = 16.5509 (6) Å

c = 15.8934 (6) Å

V = 3221.1 (2) Å3

Z = 8

Mo Kα radiation

μ = 11.75 mm−1

T = 296 K

0.36 × 0.31 × 0.27 mm

Data collection

Bruker X8 APEX Diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2009 ▶) T min = 0.512, T max = 0.640

26890 measured reflections

3559 independent reflections

2700 reflections with I > 2σ(I)

R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.051

S = 1.05

3559 reflections

138 parameters

H-atom parameters constrained

Δρmax = 0.70 e Å−3

Δρmin = −0.96 e Å−3

Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶); software used to prepare material for publication: PLATON (Spek, 2009 ▶) and publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536813018102/rz5076sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813018102/rz5076Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C7H20N2)[BiCl5]	F(000) = 1952
Mr = 518.48	Dx = 2.138 Mg m−3
Orthorhombic, Pbcn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2ab	Cell parameters from 3559 reflections
a = 12.2451 (5) Å	θ = 2.5–27.1°
b = 16.5509 (6) Å	µ = 11.75 mm−1
c = 15.8934 (6) Å	T = 296 K
V = 3221.1 (2) Å3	Block, colourless
Z = 8	0.36 × 0.31 × 0.27 mm

Bruker X8 APEX Diffractometer	3559 independent reflections
Radiation source: fine-focus sealed tube	2700 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
φ and ω scans	θmax = 27.1°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Bruker, 2009)	h = −15→15
Tmin = 0.512, Tmax = 0.640	k = −19→21
26890 measured reflections	l = −20→20

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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.051	H-atom parameters constrained
S = 1.05	w = 1/[σ2(Fo2) + (0.0185P)2 + 4.1437P] where P = (Fo2 + 2Fc2)/3
3559 reflections	(Δ/σ)max < 0.001
138 parameters	Δρmax = 0.70 e Å−3
0 restraints	Δρmin = −0.96 e Å−3

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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.

	x	y	z	Uiso*/Ueq
C1	0.6871 (4)	0.7642 (3)	0.0475 (3)	0.0677 (14)
H1A	0.7050	0.7509	0.1053	0.081*
H1B	0.6323	0.7259	0.0286	0.081*
C2	0.6390 (3)	0.8465 (2)	0.0455 (2)	0.0451 (9)
H2A	0.6214	0.8611	−0.0121	0.054*
H2B	0.6916	0.8853	0.0668	0.054*
C3	0.5365 (3)	0.8490 (2)	0.0987 (3)	0.0463 (9)
H3A	0.4841	0.8114	0.0750	0.056*
H3B	0.5547	0.8298	0.1547	0.056*
C4	0.4816 (3)	0.9305 (2)	0.1073 (3)	0.0441 (9)
H4A	0.4584	0.9489	0.0522	0.053*
H4B	0.5339	0.9693	0.1290	0.053*
C5	0.3835 (3)	0.9273 (2)	0.1654 (2)	0.0415 (9)
H5A	0.3273	0.8947	0.1389	0.050*
H5B	0.4048	0.9002	0.2169	0.050*
C6	0.3346 (3)	1.0084 (2)	0.1881 (2)	0.0401 (9)
H6A	0.3904	1.0421	0.2134	0.048*
H6B	0.3094	1.0350	0.1373	0.048*
C7	0.2416 (4)	0.9995 (2)	0.2478 (2)	0.0475 (11)
H7A	0.1834	0.9698	0.2204	0.057*
H7B	0.2655	0.9683	0.2960	0.057*
N1	0.7835 (4)	0.7542 (3)	−0.0032 (2)	0.0658 (11)
H11	0.8014	0.7021	−0.0052	0.079*
H12	0.8382	0.7822	0.0192	0.079*
H13	0.7704	0.7720	−0.0551	0.079*
N2	0.1985 (3)	1.0779 (2)	0.27729 (18)	0.0453 (8)
H21	0.1546	1.0699	0.3211	0.054*
H22	0.1612	1.1015	0.2359	0.054*
H23	0.2537	1.1097	0.2926	0.054*
Cl1	0.55628 (8)	0.15799 (5)	0.13916 (5)	0.0390 (2)
Cl2	0.29126 (8)	0.25115 (6)	0.19982 (6)	0.0504 (2)
Cl3	0.54355 (11)	0.38672 (7)	0.12014 (7)	0.0637 (3)
Cl4	0.54647 (9)	0.38534 (6)	−0.11631 (6)	0.0493 (2)
Cl5	0.29132 (8)	0.45097 (6)	−0.01712 (6)	0.0465 (2)
Bi1	0.5000	0.261494 (10)	0.2500	0.02717 (6)
Bi2	0.5000	0.5000	0.0000	0.02820 (6)

	U11	U22	U33	U12	U13	U23
C1	0.073 (3)	0.062 (3)	0.068 (3)	0.024 (3)	0.022 (3)	0.008 (2)
C2	0.047 (2)	0.043 (2)	0.045 (2)	0.0008 (18)	−0.0039 (18)	−0.0019 (17)
C3	0.052 (2)	0.040 (2)	0.046 (2)	−0.0019 (19)	0.0013 (19)	−0.0077 (18)
C4	0.052 (2)	0.035 (2)	0.046 (2)	0.0019 (17)	0.0019 (18)	−0.0005 (17)
C5	0.045 (2)	0.038 (2)	0.041 (2)	−0.0006 (17)	0.0000 (17)	0.0060 (16)
C6	0.041 (2)	0.041 (2)	0.038 (2)	−0.0072 (16)	0.0024 (18)	−0.0011 (16)
C7	0.043 (2)	0.046 (3)	0.054 (3)	0.0006 (17)	0.007 (2)	0.0091 (19)
N1	0.065 (3)	0.076 (3)	0.057 (2)	0.012 (2)	−0.002 (2)	0.0057 (19)
N2	0.0392 (17)	0.061 (2)	0.0356 (15)	−0.0007 (16)	0.0033 (14)	0.0017 (15)
Cl1	0.0461 (5)	0.0372 (5)	0.0336 (4)	−0.0012 (4)	0.0044 (4)	−0.0097 (4)
Cl2	0.0391 (5)	0.0545 (6)	0.0575 (6)	0.0042 (4)	−0.0104 (5)	0.0104 (5)
Cl3	0.0720 (7)	0.0646 (8)	0.0546 (6)	−0.0119 (6)	−0.0077 (6)	0.0313 (6)
Cl4	0.0520 (6)	0.0497 (6)	0.0463 (5)	−0.0004 (5)	0.0114 (5)	−0.0126 (5)
Cl5	0.0408 (5)	0.0531 (6)	0.0457 (5)	−0.0049 (4)	0.0064 (4)	−0.0023 (4)
Bi1	0.03136 (10)	0.02362 (10)	0.02653 (9)	0.000	0.00112 (8)	0.000
Bi2	0.03338 (10)	0.02704 (11)	0.02418 (9)	−0.00266 (8)	0.00014 (8)	0.00424 (6)

C1—N1	1.439 (6)	C7—H7A	0.9700
C1—C2	1.485 (6)	C7—H7B	0.9700
C1—H1A	0.9700	N1—H11	0.8900
C1—H1B	0.9700	N1—H12	0.8900
C2—C3	1.515 (5)	N1—H13	0.8900
C2—H2A	0.9700	N2—H21	0.8900
C2—H2B	0.9700	N2—H22	0.8900
C3—C4	1.513 (6)	N2—H23	0.8900
C3—H3A	0.9700	Cl1—Bi1	2.5520 (8)
C3—H3B	0.9700	Cl2—Bi1	2.6830 (10)
C4—C5	1.517 (5)	Cl3—Bi2	2.7287 (10)
C4—H4A	0.9700	Cl3—Bi1	2.9732 (10)
C4—H4B	0.9700	Cl4—Bi2	2.7097 (9)
C5—C6	1.512 (5)	Cl5—Bi2	2.6948 (9)
C5—H5A	0.9700	Bi1—Cl1i	2.5520 (8)
C5—H5B	0.9700	Bi1—Cl2i	2.6830 (10)
C6—C7	1.490 (5)	Bi1—Cl3i	2.9732 (10)
C6—H6A	0.9700	Bi2—Cl5ii	2.6948 (9)
C6—H6B	0.9700	Bi2—Cl4ii	2.7097 (9)
C7—N2	1.477 (5)	Bi2—Cl3ii	2.7287 (10)
N1—C1—C2	114.8 (4)	C1—N1—H12	109.5
N1—C1—H1A	108.6	H11—N1—H12	109.5
C2—C1—H1A	108.6	C1—N1—H13	109.5
N1—C1—H1B	108.6	H11—N1—H13	109.5
C2—C1—H1B	108.6	H12—N1—H13	109.5
H1A—C1—H1B	107.6	C7—N2—H21	109.5
C1—C2—C3	109.9 (3)	C7—N2—H22	109.5
C1—C2—H2A	109.7	H21—N2—H22	109.5
C3—C2—H2A	109.7	C7—N2—H23	109.5
C1—C2—H2B	109.7	H21—N2—H23	109.5
C3—C2—H2B	109.7	H22—N2—H23	109.5
H2A—C2—H2B	108.2	Bi2—Cl3—Bi1	158.39 (5)
C4—C3—C2	116.2 (3)	Cl1—Bi1—Cl1i	95.67 (4)
C4—C3—H3A	108.2	Cl1—Bi1—Cl2i	84.55 (3)
C2—C3—H3A	108.2	Cl1i—Bi1—Cl2i	90.53 (3)
C4—C3—H3B	108.2	Cl1—Bi1—Cl2	90.53 (3)
C2—C3—H3B	108.2	Cl1i—Bi1—Cl2	84.55 (3)
H3A—C3—H3B	107.4	Cl2i—Bi1—Cl2	172.69 (4)
C3—C4—C5	112.0 (3)	Cl1—Bi1—Cl3i	174.59 (3)
C3—C4—H4A	109.2	Cl1i—Bi1—Cl3i	86.58 (3)
C5—C4—H4A	109.2	Cl2i—Bi1—Cl3i	90.52 (3)
C3—C4—H4B	109.2	Cl2—Bi1—Cl3i	94.58 (4)
C5—C4—H4B	109.2	Cl1—Bi1—Cl3	86.58 (3)
H4A—C4—H4B	107.9	Cl1i—Bi1—Cl3	174.59 (3)
C6—C5—C4	115.3 (3)	Cl2i—Bi1—Cl3	94.58 (4)
C6—C5—H5A	108.4	Cl2—Bi1—Cl3	90.52 (3)
C4—C5—H5A	108.4	Cl3i—Bi1—Cl3	91.61 (5)
C6—C5—H5B	108.4	Cl5ii—Bi2—Cl5	180.0
C4—C5—H5B	108.4	Cl5ii—Bi2—Cl4ii	85.37 (3)
H5A—C5—H5B	107.5	Cl5—Bi2—Cl4ii	94.63 (3)
C7—C6—C5	111.6 (3)	Cl5ii—Bi2—Cl4	94.63 (3)
C7—C6—H6A	109.3	Cl5—Bi2—Cl4	85.37 (3)
C5—C6—H6A	109.3	Cl4ii—Bi2—Cl4	180.00 (4)
C7—C6—H6B	109.3	Cl5ii—Bi2—Cl3ii	92.81 (3)
C5—C6—H6B	109.3	Cl5—Bi2—Cl3ii	87.19 (3)
H6A—C6—H6B	108.0	Cl4ii—Bi2—Cl3ii	87.43 (3)
N2—C7—C6	112.9 (3)	Cl4—Bi2—Cl3ii	92.57 (3)
N2—C7—H7A	109.0	Cl5ii—Bi2—Cl3	87.19 (3)
C6—C7—H7A	109.0	Cl5—Bi2—Cl3	92.81 (3)
N2—C7—H7B	109.0	Cl4ii—Bi2—Cl3	92.57 (3)
C6—C7—H7B	109.0	Cl4—Bi2—Cl3	87.43 (3)
H7A—C7—H7B	107.8	Cl3ii—Bi2—Cl3	180.00 (4)
C1—N1—H11	109.5

D—H···A	D—H	H···A	D···A	D—H···A
N1—H13···Cl2ii	0.89	2.45	3.257 (4)	151
N2—H22···Cl4iii	0.89	2.37	3.222 (3)	159

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H13⋯Cl2i	0.89	2.45	3.257 (4)	151
N2—H22⋯Cl4ii	0.89	2.37	3.222 (3)	159

Symmetry codes: (i) ; (ii) .