Tetra­kis(4-meth­oxy­anilinium) hexa­chloridobismuthate(III) chloride monohydrate

Liu, M.-L.

doi:10.1107/S1600536812017096

metal-organic compounds

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Volume 68| Part 5| May 2012| Page m652

doi:10.1107/S1600536812017096

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Tetrakis(4-methoxyanilinium) hexachloridobismuthate(III) chloride monohydrate

Ming-Liang Liu ^a ^*

^aOrdered Matter Science Research Center, Southeast University, Nanjing 211189, People's Republic of China
^*Correspondence e-mail: jgsdxlml@163.com

(Received 8 April 2012; accepted 18 April 2012; online 21 April 2012)

In the crystal of the title compound, (C₇H₁₀NO)₄[BiCl₆]Cl·H₂O, the Bi^III cation is located on an inversion center and coordinated by six Cl⁻ anions in a slightly distorted octahedral geometry; the uncoordinated Cl⁻ anion and lattice water molecule are located on a twofold rotation axis. Two independent 4-methoxyanilinium cations are linked to the Bi complex, the uncoordinated Cl⁻ anion and lattice water molecule via N—H⋯Cl and N—H⋯O hydrogen bonds.

Related literature

For background literature concerning ferroelectric metal-organic complexes, see: Ye et al. (2009 ); Zhang et al. (2009 , 2010 ). For related structures, see: Liu (2011a ,b ,c ).

Experimental

Crystal data

(C₇H₁₀NO)₄[BiCl₆]Cl·H₂O
M_r = 971.79
Monoclinic, C 2/c
a = 25.806 (5) Å
b = 7.7081 (15) Å
c = 19.550 (4) Å
β = 104.27 (3)°
V = 3768.8 (13) Å³
Z = 4
Mo Kα radiation
μ = 5.22 mm⁻¹
T = 293 K
0.21 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ) T_min = 0.350, T_max = 0.364
18912 measured reflections
4320 independent reflections
3223 reflections with I > 2σ(I)
R_int = 0.055

Refinement

R[F² > 2σ(F²)] = 0.031
wR(F²) = 0.065
S = 1.07
4320 reflections
212 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.46 e Å⁻³
Δρ_min = −0.89 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯O3	0.89	2.01	2.862 (5)	161
N1—H1B⋯Cl2	0.89	2.41	3.224 (4)	152
N1—H1C⋯Cl1	0.89	2.37	3.231 (4)	165
N2—H2A⋯Cl3ⁱ	0.89	2.67	3.411 (4)	141
N2—H2A⋯Cl2ⁱⁱ	0.89	2.68	3.330 (4)	131
N2—H2B⋯Cl4ⁱⁱⁱ	0.89	2.78	3.312 (3)	120
N2—H2B⋯Cl3^iv	0.89	2.83	3.648 (4)	153
N2—H2C⋯Cl1ⁱⁱⁱ	0.89	2.55	3.418 (4)	167
O3—H3B⋯Cl1^v	0.85 (1)	2.70 (2)	3.202 (6)	119 (2)
Symmetry codes: (i) $[x+{\script{1\over 2}}, y-{\script{1\over 2}}, z]$ ; (ii) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]$ ; (iii) $[x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ ; (iv) $[-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z]$ ; (v) x, y+1, z.

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812017096/xu5513sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812017096/xu5513Isup2.hkl

checkCIF report

Comment top

Recently much attention has been devoted to simple molecular-ionic compounds containing inorganic and organic ions due to the tunability of their special structural features and their potential ferroelectrics property. Ferroelectric materials that exhibit reversible electric polarization in response to an external electric field have found many applications such as nonvolatile memory storage, electronics and optics. The freezing of a certain functional group at low temperature forces significant orientational motions of the guest molecules and thus induces the formation of the ferroelectric phase. (Zhang et al. 2009; Ye et al. 2009; Zhang et al. 2010). In our laboratory, the title compound has been synthesized and its crystal structure is herein reported.

The title compound, [(C₇H₁₀NO)₄BiCl₆]Cl.H₂O, has an asymmetric unit that consists of two 4-methoxyanilinium cations, half an octahedral hexachloridobismuthate anion, a chloride anion, and half a water molecule (Fig 1). The non-hydrogen atoms of C₇H₁₀NO cations are nearly coplanar, the bismuth atom is coordinated by six chlorides, forming a distorted octahedron, the average Bi—Cl bond distances range from 2.6881 (12) Å to 2.6926 (10) Å, the Cl—Bi—Cl angles range from 85.67 (4)°to 180.00 (7)°. In the crystal, numerous N—H^···Cl, N—H^···O, O—H^···Cl and bifurcated N—H^···(Cl,Cl) hydrogen bonds link the components to a form layer structure which is parallel to bc plane (Fig 2).

Related literature top

For background literature concerning ferroelectric metal-organic complexes, see: Ye et al. (2009); Zhang et al. (2009, 2010). For related structures, see: Liu (2011a,b,c).

Experimental top

4-Methoxylbenzenamine (3.69 g, 0.03 mol) was firstly dissolved in 30 ml ethanol, to which 1.1 g (0.03 mol) of hydrochloric acid was then added to afford the solution, then 3.15 g (0.01 mol) bisumth chloride was dissolved in 20 ml ethanol which was added hydrochloric acid, at last, mixed the above solution without any precipitation under stirring at the ambient temperature. Single crystals suitable for X-ray structure analysis were obtained by the slow evaporation of the above solution after 6 days in air.

The dielectric constant of the compound as a function of temperature indicates that the permittivity is basically temperature-independent (ε = C/(T–T₀)), suggesting that this compound is not ferroelectric or there may be no distinct phase transition occurring within the measured temperature within the measured temperature (below the melting point).

Computing details top

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008.

Figures top

	Fig. 1. The molecular structure of the title compound, showing the atomic numbering scheme with 30% probability displacement ellipsoids.
	Fig. 2. Crystal structure of the title compound with view along the b axis. Intermolecular interactions are shown as dashed lines.

Tetrakis(4-methoxyanilinium) hexachloridobismuthate(III) chloride monohydrate top

Crystal data top

(C₇H₁₀NO)₄[BiCl₆]Cl·H₂O	F(000) = 1920
M_r = 971.79	D_x = 1.713 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3223 reflections
a = 25.806 (5) Å	θ = 0–26°
b = 7.7081 (15) Å	µ = 5.22 mm⁻¹
c = 19.550 (4) Å	T = 293 K
β = 104.27 (3)°	Block, colourless
V = 3768.8 (13) Å³	0.21 × 0.20 × 0.20 mm
Z = 4

Data collection top

Rigaku SCXmini diffractometer	4320 independent reflections
Radiation source: fine-focus sealed tube	3223 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.055
CCD_Profile_fitting scans	θ_max = 27.5°, θ_min = 3.0°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	h = −33→33
T_min = 0.350, T_max = 0.364	k = −10→10
18912 measured reflections	l = −25→25

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.065	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ²(F_o²) + (0.0215P)²] where P = (F_o² + 2F_c²)/3
4320 reflections	(Δ/σ)_max < 0.001
212 parameters	Δρ_max = 0.46 e Å⁻³
2 restraints	Δρ_min = −0.89 e Å⁻³

Crystal data top

(C₇H₁₀NO)₄[BiCl₆]Cl·H₂O	V = 3768.8 (13) Å³
M_r = 971.79	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 25.806 (5) Å	µ = 5.22 mm⁻¹
b = 7.7081 (15) Å	T = 293 K
c = 19.550 (4) Å	0.21 × 0.20 × 0.20 mm
β = 104.27 (3)°

Data collection top

Rigaku SCXmini diffractometer	4320 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	3223 reflections with I > 2σ(I)
T_min = 0.350, T_max = 0.364	R_int = 0.055
18912 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.031	2 restraints
wR(F²) = 0.065	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	Δρ_max = 0.46 e Å⁻³
4320 reflections	Δρ_min = −0.89 e Å⁻³
212 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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	U_iso*/U_eq
O1	0.28804 (11)	0.4079 (3)	0.34243 (14)	0.0518 (7)
N1	0.07004 (13)	0.4069 (5)	0.21893 (18)	0.0586 (9)
H1A	0.0550	0.5033	0.2301	0.070*
H1B	0.0642	0.3995	0.1722	0.070*
H1C	0.0558	0.3152	0.2350	0.070*
C1	0.32410 (19)	0.5181 (5)	0.3189 (3)	0.0680 (14)
H1D	0.3126	0.6364	0.3197	0.102*
H1E	0.3249	0.4869	0.2716	0.102*
H1F	0.3592	0.5057	0.3494	0.102*
C2	0.21434 (17)	0.5117 (4)	0.2491 (2)	0.0421 (9)
H2	0.2365	0.5776	0.2283	0.050*
C3	0.16029 (17)	0.5079 (4)	0.2199 (2)	0.0454 (9)
H3	0.1458	0.5709	0.1790	0.055*
C4	0.12749 (15)	0.4115 (5)	0.2505 (2)	0.0404 (9)
C5	0.14777 (17)	0.3185 (5)	0.3107 (2)	0.0482 (10)
H5	0.1253	0.2536	0.3313	0.058*
C6	0.20162 (17)	0.3228 (5)	0.33989 (19)	0.0483 (10)
H6	0.2156	0.2606	0.3811	0.058*
C7	0.23587 (15)	0.4174 (4)	0.30985 (19)	0.0358 (8)
O2	0.23658 (13)	0.3700 (4)	0.07934 (16)	0.0683 (9)
N2	0.44637 (15)	0.5170 (4)	0.0738 (2)	0.0606 (10)
H2A	0.4616	0.4253	0.0590	0.073*
H2B	0.4469	0.6062	0.0450	0.073*
H2C	0.4644	0.5447	0.1173	0.073*
C8	0.1924 (2)	0.4511 (6)	0.0331 (3)	0.0781 (16)
H8A	0.1928	0.4259	−0.0149	0.117*
H8B	0.1945	0.5742	0.0405	0.117*
H8C	0.1598	0.4081	0.0422	0.117*
C9	0.32753 (18)	0.3409 (5)	0.1260 (2)	0.0548 (11)
H9	0.3199	0.2725	0.1614	0.066*
C10	0.37990 (17)	0.3753 (5)	0.1258 (2)	0.0545 (11)
H10	0.4075	0.3304	0.1613	0.065*
C11	0.35099 (19)	0.5412 (5)	0.0212 (2)	0.0500 (11)
H11	0.3588	0.6095	−0.0141	0.060*
C12	0.28621 (17)	0.4080 (5)	0.0733 (2)	0.0450 (10)
C13	0.29834 (18)	0.5055 (4)	0.0210 (2)	0.0500 (10)
H13	0.2709	0.5483	−0.0153	0.060*
C14	0.39129 (17)	0.4754 (4)	0.0737 (2)	0.0425 (9)
Bi1	0.0000	0.5000	0.0000	0.03569 (7)
Cl2	0.06254 (4)	0.23985 (12)	0.06560 (5)	0.0521 (3)
Cl3	0.05299 (4)	0.74622 (13)	0.08758 (6)	0.0610 (3)
Cl4	−0.05859 (5)	0.44282 (15)	0.09398 (6)	0.0623 (3)
O3	0.0000	0.6668 (7)	0.2500	0.112 (2)
Cl1	0.0000	0.0822 (2)	0.2500	0.0579 (4)
H3B	0.0155 (18)	0.741 (2)	0.230 (3)	0.15 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O1	0.0405 (18)	0.0500 (16)	0.0567 (17)	−0.0059 (14)	−0.0034 (14)	0.0099 (14)
N1	0.038 (2)	0.071 (2)	0.068 (2)	−0.0017 (19)	0.0168 (19)	−0.007 (2)
C1	0.040 (3)	0.066 (3)	0.090 (4)	−0.011 (2)	0.000 (3)	0.011 (2)
C2	0.042 (2)	0.042 (2)	0.042 (2)	−0.0055 (18)	0.0093 (18)	0.0060 (18)
C3	0.043 (3)	0.049 (2)	0.042 (2)	0.0016 (19)	0.0056 (18)	0.0119 (19)
C4	0.032 (2)	0.043 (2)	0.049 (2)	−0.0043 (18)	0.0152 (19)	−0.0112 (19)
C5	0.050 (3)	0.047 (2)	0.055 (3)	−0.0081 (19)	0.027 (2)	0.001 (2)
C6	0.063 (3)	0.047 (2)	0.036 (2)	−0.002 (2)	0.012 (2)	0.0077 (18)
C7	0.039 (2)	0.0319 (19)	0.034 (2)	−0.0023 (17)	0.0050 (18)	−0.0041 (16)
O2	0.047 (2)	0.083 (2)	0.078 (2)	−0.0194 (17)	0.0213 (18)	−0.0023 (18)
N2	0.049 (2)	0.054 (2)	0.081 (3)	−0.0016 (16)	0.021 (2)	−0.0125 (17)
C8	0.045 (3)	0.082 (3)	0.107 (4)	−0.006 (3)	0.018 (3)	−0.021 (3)
C9	0.059 (3)	0.052 (2)	0.055 (3)	−0.010 (2)	0.016 (2)	0.010 (2)
C10	0.054 (3)	0.047 (2)	0.052 (3)	−0.001 (2)	−0.006 (2)	0.006 (2)
C11	0.056 (3)	0.047 (2)	0.053 (3)	0.0013 (19)	0.025 (2)	0.0025 (19)
C12	0.047 (3)	0.040 (2)	0.051 (3)	−0.010 (2)	0.019 (2)	−0.0103 (19)
C13	0.049 (3)	0.054 (2)	0.046 (2)	0.013 (2)	0.010 (2)	0.002 (2)
C14	0.040 (2)	0.034 (2)	0.055 (2)	−0.0028 (17)	0.015 (2)	−0.0067 (18)
Bi1	0.02767 (12)	0.03032 (11)	0.04936 (13)	0.00127 (9)	0.01004 (9)	0.00439 (10)
Cl2	0.0438 (6)	0.0471 (5)	0.0623 (6)	0.0162 (5)	0.0072 (5)	0.0057 (5)
Cl3	0.0500 (7)	0.0438 (6)	0.0786 (8)	−0.0087 (5)	−0.0047 (6)	−0.0071 (5)
Cl4	0.0548 (8)	0.0659 (6)	0.0779 (8)	−0.0033 (5)	0.0387 (6)	0.0005 (6)
O3	0.078 (4)	0.056 (3)	0.217 (7)	0.000	0.063 (5)	0.000
Cl1	0.0523 (10)	0.0516 (8)	0.0652 (10)	0.000	0.0056 (8)	0.000

Geometric parameters (Å, º) top

O1—C7	1.342 (4)	N2—H2B	0.8910
O1—C1	1.418 (5)	N2—H2C	0.8890
N1—C4	1.459 (5)	C8—H8A	0.9600
N1—H1A	0.8902	C8—H8B	0.9600
N1—H1B	0.8898	C8—H8C	0.9600
N1—H1C	0.8890	C9—C10	1.378 (5)
C1—H1D	0.9600	C9—C12	1.387 (5)
C1—H1E	0.9600	C9—H9	0.9300
C1—H1F	0.9600	C10—C14	1.368 (5)
C2—C3	1.371 (5)	C10—H10	0.9300
C2—C7	1.386 (5)	C11—C14	1.365 (6)
C2—H2	0.9300	C11—C13	1.385 (6)
C3—C4	1.370 (5)	C11—H11	0.9300
C3—H3	0.9300	C12—C13	1.367 (5)
C4—C5	1.367 (5)	C13—H13	0.9300
C5—C6	1.367 (5)	Bi1—Cl4ⁱ	2.6881 (12)
C5—H5	0.9300	Bi1—Cl4	2.6881 (12)
C6—C7	1.383 (5)	Bi1—Cl3	2.6925 (11)
C6—H6	0.9300	Bi1—Cl3ⁱ	2.6925 (11)
O2—C12	1.347 (4)	Bi1—Cl2	2.6927 (10)
O2—C8	1.414 (5)	Bi1—Cl2ⁱ	2.6927 (10)
N2—C14	1.456 (5)	O3—H3B	0.846 (10)
N2—H2A	0.8910

C7—O1—C1	118.4 (3)	O2—C8—H8B	109.5
C4—N1—H1A	109.5	H8A—C8—H8B	109.5
C4—N1—H1B	109.4	O2—C8—H8C	109.5
H1A—N1—H1B	109.4	H8A—C8—H8C	109.5
C4—N1—H1C	109.6	H8B—C8—H8C	109.5
H1A—N1—H1C	109.5	C10—C9—C12	120.1 (4)
H1B—N1—H1C	109.4	C10—C9—H9	120.0
O1—C1—H1D	109.5	C12—C9—H9	120.0
O1—C1—H1E	109.5	C14—C10—C9	120.1 (4)
H1D—C1—H1E	109.5	C14—C10—H10	119.9
O1—C1—H1F	109.5	C9—C10—H10	119.9
H1D—C1—H1F	109.5	C14—C11—C13	119.6 (4)
H1E—C1—H1F	109.5	C14—C11—H11	120.2
C3—C2—C7	119.9 (4)	C13—C11—H11	120.2
C3—C2—H2	120.1	O2—C12—C13	125.7 (4)
C7—C2—H2	120.1	O2—C12—C9	115.3 (4)
C4—C3—C2	120.3 (4)	C13—C12—C9	119.0 (4)
C4—C3—H3	119.9	C12—C13—C11	120.8 (4)
C2—C3—H3	119.9	C12—C13—H13	119.6
C5—C4—C3	120.9 (4)	C11—C13—H13	119.6
C5—C4—N1	119.0 (4)	C11—C14—C10	120.4 (4)
C3—C4—N1	120.1 (4)	C11—C14—N2	118.8 (4)
C6—C5—C4	118.8 (4)	C10—C14—N2	120.8 (4)
C6—C5—H5	120.6	Cl4ⁱ—Bi1—Cl4	180.00 (3)
C4—C5—H5	120.6	Cl4ⁱ—Bi1—Cl3	92.06 (4)
C5—C6—C7	121.7 (4)	Cl4—Bi1—Cl3	87.94 (4)
C5—C6—H6	119.1	Cl4ⁱ—Bi1—Cl3ⁱ	87.94 (4)
C7—C6—H6	119.1	Cl4—Bi1—Cl3ⁱ	92.06 (4)
O1—C7—C6	116.2 (3)	Cl3—Bi1—Cl3ⁱ	180.00 (7)
O1—C7—C2	125.4 (3)	Cl4ⁱ—Bi1—Cl2	94.33 (4)
C6—C7—C2	118.5 (4)	Cl4—Bi1—Cl2	85.67 (4)
C12—O2—C8	118.8 (4)	Cl3—Bi1—Cl2	94.08 (4)
C14—N2—H2A	109.5	Cl3ⁱ—Bi1—Cl2	85.92 (4)
C14—N2—H2B	109.6	Cl4ⁱ—Bi1—Cl2ⁱ	85.67 (4)
H2A—N2—H2B	109.3	Cl4—Bi1—Cl2ⁱ	94.33 (4)
C14—N2—H2C	109.6	Cl3—Bi1—Cl2ⁱ	85.92 (4)
H2A—N2—H2C	109.4	Cl3ⁱ—Bi1—Cl2ⁱ	94.08 (4)
H2B—N2—H2C	109.5	Cl2—Bi1—Cl2ⁱ	180.00 (6)
O2—C8—H8A	109.5

C7—C2—C3—C4	0.2 (5)	C12—C9—C10—C14	−0.2 (6)
C2—C3—C4—C5	0.4 (6)	C8—O2—C12—C13	−7.6 (6)
C2—C3—C4—N1	−179.6 (3)	C8—O2—C12—C9	172.2 (4)
C3—C4—C5—C6	−0.2 (6)	C10—C9—C12—O2	−178.5 (3)
N1—C4—C5—C6	179.8 (3)	C10—C9—C12—C13	1.2 (6)
C4—C5—C6—C7	−0.5 (6)	O2—C12—C13—C11	177.9 (4)
C1—O1—C7—C6	−172.6 (4)	C9—C12—C13—C11	−1.8 (6)
C1—O1—C7—C2	8.1 (5)	C14—C11—C13—C12	1.3 (6)
C5—C6—C7—O1	−178.4 (3)	C13—C11—C14—C10	−0.2 (6)
C5—C6—C7—C2	1.0 (5)	C13—C11—C14—N2	−178.9 (3)
C3—C2—C7—O1	178.5 (3)	C9—C10—C14—C11	−0.3 (6)
C3—C2—C7—C6	−0.8 (5)	C9—C10—C14—N2	178.3 (3)

Symmetry code: (i) −x, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O3	0.89	2.01	2.862 (5)	161
N1—H1B···Cl2	0.89	2.41	3.224 (4)	152
N1—H1C···Cl1	0.89	2.37	3.231 (4)	165
N2—H2A···Cl3ⁱⁱ	0.89	2.67	3.411 (4)	141
N2—H2A···Cl2ⁱⁱⁱ	0.89	2.68	3.330 (4)	131
N2—H2B···Cl4^iv	0.89	2.78	3.312 (3)	120
N2—H2B···Cl3^v	0.89	2.83	3.648 (4)	153
N2—H2C···Cl1^iv	0.89	2.55	3.418 (4)	167
O3—H3B···Cl1^vi	0.85 (1)	2.70 (2)	3.202 (6)	119 (2)

Symmetry codes: (ii) x+1/2, y−1/2, z; (iii) −x+1/2, −y+1/2, −z; (iv) x+1/2, y+1/2, z; (v) −x+1/2, −y+3/2, −z; (vi) x, y+1, z.

Experimental details

Crystal data
Chemical formula	(C₇H₁₀NO)₄[BiCl₆]Cl·H₂O
M_r	971.79
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	25.806 (5), 7.7081 (15), 19.550 (4)
β (°)	104.27 (3)
V (Å³)	3768.8 (13)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.22
Crystal size (mm)	0.21 × 0.20 × 0.20

Data collection
Diffractometer	Rigaku SCXmini diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2005)
T_min, T_max	0.350, 0.364
No. of measured, independent and observed [I > 2σ(I)] reflections	18912, 4320, 3223
R_int	0.055
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.031, 0.065, 1.07
No. of reflections	4320
No. of parameters	212
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.46, −0.89

Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), SHELXTL (Sheldrick, 2008.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O3	0.89	2.01	2.862 (5)	160.7
N1—H1B···Cl2	0.89	2.41	3.224 (4)	151.9
N1—H1C···Cl1	0.89	2.37	3.231 (4)	164.7
N2—H2A···Cl3ⁱ	0.89	2.67	3.411 (4)	141.2
N2—H2A···Cl2ⁱⁱ	0.89	2.68	3.330 (4)	130.5
N2—H2B···Cl4ⁱⁱⁱ	0.89	2.78	3.312 (3)	119.5
N2—H2B···Cl3^iv	0.89	2.83	3.648 (4)	153.2
N2—H2C···Cl1ⁱⁱⁱ	0.89	2.55	3.418 (4)	167.0
O3—H3B···Cl1^v	0.846 (10)	2.70 (2)	3.202 (6)	119 (2)

Symmetry codes: (i) x+1/2, y−1/2, z; (ii) −x+1/2, −y+1/2, −z; (iii) x+1/2, y+1/2, z; (iv) −x+1/2, −y+3/2, −z; (v) x, y+1, z.

Acknowledgements

The author thanks an anonymous adivisor from the Ordered Matter Science Research Centre, Southeast University, for great help in the revision of this paper.

References

Liu, M.-L. (2011a). Acta Cryst. E67, m1622. Web of Science CSD CrossRef IUCr Journals Google Scholar
Liu, M.-L. (2011b). Acta Cryst. E67, m1812. Web of Science CSD CrossRef IUCr Journals Google Scholar
Liu, M.-L. (2011c). Acta Cryst. E67, m1827. Web of Science CSD CrossRef IUCr Journals Google Scholar
Rigaku (2005). CrystalClear. Rigaku Corporation, Tokyo, Japan. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Ye, H.-Y., Fu, D.-W., Zhang, Y., Zhang, W., Xiong, R.-G. & Huang, S.-P. (2009). J. Am. Chem. Soc. 131, 42–43. Web of Science CSD CrossRef PubMed CAS Google Scholar
Zhang, W., Chen, L.-Z., Xiong, R.-G., Nakamura, T. & Huang, S.-P. (2009). J. Am. Chem. Soc. 131, 12544–12545. Web of Science CSD CrossRef PubMed CAS Google Scholar
Zhang, W., Ye, H.-Y., Cai, H.-L., Ge, J.-Z., Xiong, R.-G. & Huang, S.-P. (2010). J. Am. Chem. Soc. 132, 7300–7302. Web of Science CSD CrossRef CAS PubMed Google Scholar

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Volume 68| Part 5| May 2012| Page m652

doi:10.1107/S1600536812017096

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Tetra­kis(4-meth­­oxy­anilinium) hexa­chloridobismuthate(III) chloride monohydrate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Tetrakis(4-methoxyanilinium) hexachloridobismuthate(III) chloride monohydrate