Literature DB >> 22199505

Bis(piperazine-1,4-diium) hexa-chlorido-bismuthate(III) chloride monohydrate.

Yu-Hua Gao¹, Xiao-Jia Liu, Lei Sun, Wen-Jun Le.

Abstract

The crystal structure of the title compound, (C(4)H(12)N(2))(2)[BiCl(6)]Cl·H(2)O, consists of piperazinediium cations, [BiCl(6)](3-) anions, Cl(-) anions and uncoordinated water mol-ecules. The Bi(III) cation is coordinated by six Cl(-) anions in a slightly distorted octa-hedral geometry. The diprotonated piperazine ring adopts a chair conformation. In the crystal, extensive inter-molecular N-H⋯Cl, N-H⋯O and O-H⋯Cl hydrogen bonds occur.

Entities: CellLine Chemical Disease Species

Year: 2011 PMID： 22199505 PMCID： PMC3238614 DOI： 10.1107/S1600536811045594

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For related structures, see: Wu et al. (2005 ▶); Fu et al. (2005 ▶)

Experimental

Crystal data

(C4H12N2)2[BiCl6]Cl·H2O M = 651.46 Monoclinic, a = 11.085 (3) Å b = 16.642 (4) Å c = 11.862 (3) Å β = 98.997 (3)° V = 2161.3 (10) Å3 Z = 4 Mo Kα radiation μ = 9.03 mm−1 T = 296 K 0.20 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T min = 0.266, T max = 0.266 12000 measured reflections 4108 independent reflections 3341 reflections with I > 2σ(I) R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 0.061 S = 1.03 4108 reflections 197 parameters 3 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.66 e Å−3 Δρmin = −0.54 e Å−3 Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811045594/xu5366sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811045594/xu5366Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C₄H₁₂N₂)₂[BiCl₆]Cl·H₂O	F(000) = 1248
M_r = 651.46	D_x = 2.002 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3341 reflections
a = 11.085 (3) Å	θ = 1.9–26°
b = 16.642 (4) Å	µ = 9.03 mm⁻¹
c = 11.862 (3) Å	T = 296 K
β = 98.997 (3)°	Block, colorless
V = 2161.3 (10) Å³	0.20 × 0.20 × 0.20 mm
Z = 4

Rigaku SCXmini diffractometer	4108 independent reflections
Radiation source: fine-focus sealed tube	3341 reflections with I > 2σ(I)
graphite	R_int = 0.041
Detector resolution: 13.6612 pixels mm^-1	θ_max = 26.0°, θ_min = 1.9°
ω scans	h = −13→13
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	k = −17→20
T_min = 0.266, T_max = 0.266	l = −13→14
12000 measured reflections

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)] = 0.027	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.061	w = 1/[σ²(F_o²) + (0.0226P)²] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.002
4108 reflections	Δρ_max = 0.66 e Å⁻³
197 parameters	Δρ_min = −0.54 e Å⁻³
3 restraints	Extinction correction: SHELXTL (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00472 (14)

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.

	x	y	z	U_iso*/U_eq
Bi1	0.740018 (15)	0.092026 (11)	0.807034 (15)	0.02849 (9)
Cl2	0.79302 (15)	0.11877 (12)	0.60299 (13)	0.0670 (5)
C6	0.9370 (5)	0.3286 (3)	0.6818 (4)	0.0390 (13)
H6A	0.8528	0.3112	0.6758	0.047*
H6B	0.9707	0.3059	0.6181	0.047*
Cl3	0.97693 (11)	0.09950 (7)	0.90506 (12)	0.0394 (3)
Cl4	0.68343 (11)	0.05928 (8)	1.02452 (11)	0.0376 (3)
Cl6	0.70154 (12)	0.24996 (8)	0.83713 (12)	0.0442 (3)
Cl5	0.49653 (12)	0.07440 (9)	0.74387 (13)	0.0491 (4)
C4	0.4452 (5)	0.1743 (3)	1.0987 (5)	0.0476 (15)
H4A	0.5070	0.1454	1.1500	0.057*
H4B	0.3783	0.1868	1.1397	0.057*
C3	0.4981 (5)	0.2503 (3)	1.0608 (5)	0.0459 (14)
H3A	0.5253	0.2841	1.1265	0.055*
H3B	0.5682	0.2380	1.0241	0.055*
N1	0.4004 (4)	0.1236 (3)	0.9985 (4)	0.0483 (12)
H1A	0.3673	0.0784	1.0221	0.058*
H1D	0.4638	0.1094	0.9638	0.058*
N2	0.4051 (4)	0.2935 (3)	0.9799 (4)	0.0485 (12)
H2A	0.4377	0.3391	0.9570	0.058*
H2D	0.3417	0.3069	1.0151	0.058*
C1	0.3073 (5)	0.1661 (3)	0.9150 (5)	0.0474 (15)
H1B	0.2357	0.1777	0.9497	0.057*
H1C	0.2827	0.1322	0.8489	0.057*
C2	0.3612 (5)	0.2428 (3)	0.8790 (5)	0.0474 (15)
H2B	0.4288	0.2306	0.8388	0.057*
H2C	0.3000	0.2719	0.8273	0.057*
Cl1	0.76430 (12)	−0.06850 (9)	0.77947 (15)	0.0542 (4)
N4	0.9416 (4)	0.4179 (2)	0.6760 (4)	0.0348 (10)
H4C	1.0193	0.4338	0.6764	0.042*
H4D	0.8970	0.4347	0.6103	0.042*
N3	0.9625 (4)	0.3368 (3)	0.8914 (4)	0.0459 (12)
H3C	0.8856	0.3203	0.8937	0.055*
H3D	1.0096	0.3206	0.9561	0.055*
C8	0.9648 (5)	0.4261 (3)	0.8847 (5)	0.0487 (15)
H8A	1.0487	0.4443	0.8911	0.058*
H8B	0.9301	0.4487	0.9479	0.058*
C7	0.8937 (5)	0.4550 (3)	0.7740 (5)	0.0474 (14)
H7A	0.8082	0.4411	0.7706	0.057*
H7B	0.8998	0.5130	0.7695	0.057*
C5	1.0076 (5)	0.2991 (3)	0.7909 (5)	0.0439 (14)
H5A	1.0934	0.3118	0.7933	0.053*
H5B	0.9998	0.2411	0.7950	0.053*
Cl7	0.16914 (12)	0.31589 (10)	0.09392 (12)	0.0537 (4)
O1	0.5352 (5)	0.4184 (3)	0.9159 (6)	0.099 (2)
H9A	0.610 (3)	0.425 (4)	0.941 (6)	0.119*
H9B	0.519 (6)	0.452 (4)	0.862 (5)	0.119*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Bi1	0.02867 (12)	0.02880 (13)	0.02927 (13)	0.00082 (8)	0.00847 (8)	0.00086 (9)
Cl2	0.0689 (11)	0.0968 (13)	0.0406 (9)	0.0061 (9)	0.0256 (8)	0.0120 (9)
C6	0.058 (4)	0.030 (3)	0.031 (3)	−0.008 (3)	0.013 (3)	−0.001 (2)
Cl3	0.0340 (6)	0.0433 (8)	0.0412 (8)	0.0000 (6)	0.0062 (6)	0.0025 (6)
Cl4	0.0387 (7)	0.0423 (8)	0.0326 (7)	−0.0034 (6)	0.0080 (6)	0.0011 (6)
Cl6	0.0412 (7)	0.0353 (8)	0.0590 (10)	−0.0036 (6)	0.0167 (7)	−0.0065 (7)
Cl5	0.0344 (7)	0.0585 (10)	0.0538 (9)	0.0017 (6)	0.0044 (6)	−0.0146 (7)
C4	0.045 (3)	0.060 (4)	0.040 (4)	0.001 (3)	0.014 (3)	0.002 (3)
C3	0.041 (3)	0.054 (4)	0.043 (4)	−0.009 (3)	0.008 (3)	−0.011 (3)
N1	0.042 (3)	0.032 (3)	0.075 (4)	−0.007 (2)	0.021 (3)	−0.005 (3)
N2	0.057 (3)	0.035 (3)	0.059 (3)	−0.003 (2)	0.027 (3)	−0.002 (2)
C1	0.034 (3)	0.056 (4)	0.050 (4)	−0.005 (3)	0.003 (3)	−0.017 (3)
C2	0.045 (3)	0.055 (4)	0.044 (4)	0.006 (3)	0.013 (3)	0.007 (3)
Cl1	0.0409 (8)	0.0343 (8)	0.0903 (12)	0.0001 (6)	0.0192 (8)	−0.0105 (8)
N4	0.034 (2)	0.040 (3)	0.030 (3)	−0.0021 (19)	0.0023 (19)	0.008 (2)
N3	0.038 (3)	0.067 (3)	0.031 (3)	−0.014 (2)	0.000 (2)	0.019 (2)
C8	0.053 (4)	0.065 (4)	0.031 (3)	−0.018 (3)	0.015 (3)	−0.009 (3)
C7	0.053 (4)	0.044 (4)	0.047 (4)	0.001 (3)	0.016 (3)	−0.008 (3)
C5	0.044 (3)	0.040 (3)	0.049 (4)	0.000 (3)	0.012 (3)	0.012 (3)
Cl7	0.0389 (8)	0.0854 (12)	0.0366 (9)	0.0057 (7)	0.0050 (6)	−0.0004 (8)
O1	0.079 (4)	0.073 (4)	0.139 (6)	−0.016 (3)	−0.002 (4)	0.062 (3)

Bi1—Cl2	2.6164 (16)	N2—H2D	0.9000
Bi1—Cl6	2.6954 (14)	C1—C2	1.499 (7)
Bi1—Cl5	2.7019 (14)	C1—H1B	0.9700
Bi1—Cl3	2.7036 (14)	C1—H1C	0.9700
Bi1—Cl1	2.7099 (15)	C2—H2B	0.9700
Bi1—Cl4	2.8021 (14)	C2—H2C	0.9700
C6—C5	1.488 (7)	N4—C7	1.486 (6)
C6—N4	1.488 (6)	N4—H4C	0.9000
C6—H6A	0.9700	N4—H4D	0.9000
C6—H6B	0.9700	N3—C8	1.488 (7)
C4—N1	1.479 (6)	N3—C5	1.500 (7)
C4—C3	1.493 (7)	N3—H3C	0.9000
C4—H4A	0.9700	N3—H3D	0.9000
C4—H4B	0.9700	C8—C7	1.502 (7)
C3—N2	1.480 (7)	C8—H8A	0.9700
C3—H3A	0.9700	C8—H8B	0.9700
C3—H3B	0.9700	C7—H7A	0.9700
N1—C1	1.492 (7)	C7—H7B	0.9700
N1—H1A	0.9000	C5—H5A	0.9700
N1—H1D	0.9000	C5—H5B	0.9700
N2—C2	1.483 (7)	O1—H9A	0.844 (19)
N2—H2A	0.9000	O1—H9B	0.854 (19)

Cl2—Bi1—Cl6	91.13 (5)	H2A—N2—H2D	108.1
Cl2—Bi1—Cl5	96.95 (5)	N1—C1—C2	109.1 (4)
Cl6—Bi1—Cl5	88.32 (4)	N1—C1—H1B	109.9
Cl2—Bi1—Cl3	92.66 (5)	C2—C1—H1B	109.9
Cl6—Bi1—Cl3	93.52 (4)	N1—C1—H1C	109.9
Cl5—Bi1—Cl3	170.17 (4)	C2—C1—H1C	109.9
Cl2—Bi1—Cl1	90.87 (6)	H1B—C1—H1C	108.3
Cl6—Bi1—Cl1	176.40 (4)	N2—C2—C1	110.5 (4)
Cl5—Bi1—Cl1	88.47 (4)	N2—C2—H2B	109.6
Cl3—Bi1—Cl1	89.38 (4)	C1—C2—H2B	109.6
Cl2—Bi1—Cl4	178.58 (5)	N2—C2—H2C	109.6
Cl6—Bi1—Cl4	90.28 (4)	C1—C2—H2C	109.6
Cl5—Bi1—Cl4	82.90 (4)	H2B—C2—H2C	108.1
Cl3—Bi1—Cl4	87.44 (4)	C7—N4—C6	111.1 (4)
Cl1—Bi1—Cl4	87.72 (5)	C7—N4—H4C	109.4
C5—C6—N4	110.7 (4)	C6—N4—H4C	109.4
C5—C6—H6A	109.5	C7—N4—H4D	109.4
N4—C6—H6A	109.5	C6—N4—H4D	109.4
C5—C6—H6B	109.5	H4C—N4—H4D	108.0
N4—C6—H6B	109.5	C8—N3—C5	111.4 (4)
H6A—C6—H6B	108.1	C8—N3—H3C	109.3
N1—C4—C3	109.9 (4)	C5—N3—H3C	109.3
N1—C4—H4A	109.7	C8—N3—H3D	109.3
C3—C4—H4A	109.7	C5—N3—H3D	109.3
N1—C4—H4B	109.7	H3C—N3—H3D	108.0
C3—C4—H4B	109.7	N3—C8—C7	110.8 (4)
H4A—C4—H4B	108.2	N3—C8—H8A	109.5
N2—C3—C4	109.9 (4)	C7—C8—H8A	109.5
N2—C3—H3A	109.7	N3—C8—H8B	109.5
C4—C3—H3A	109.7	C7—C8—H8B	109.5
N2—C3—H3B	109.7	H8A—C8—H8B	108.1
C4—C3—H3B	109.7	N4—C7—C8	110.3 (4)
H3A—C3—H3B	108.2	N4—C7—H7A	109.6
C4—N1—C1	112.0 (4)	C8—C7—H7A	109.6
C4—N1—H1A	109.2	N4—C7—H7B	109.6
C1—N1—H1A	109.2	C8—C7—H7B	109.6
C4—N1—H1D	109.2	H7A—C7—H7B	108.1
C1—N1—H1D	109.2	C6—C5—N3	110.9 (4)
H1A—N1—H1D	107.9	C6—C5—H5A	109.4
C3—N2—C2	110.7 (4)	N3—C5—H5A	109.4
C3—N2—H2A	109.5	C6—C5—H5B	109.4
C2—N2—H2A	109.5	N3—C5—H5B	109.4
C3—N2—H2D	109.5	H5A—C5—H5B	108.0
C2—N2—H2D	109.5	H9A—O1—H9B	105 (3)

N1—C4—C3—N2	57.7 (6)	C5—C6—N4—C7	−57.7 (5)
C3—C4—N1—C1	−57.7 (6)	C5—N3—C8—C7	55.3 (6)
C4—C3—N2—C2	−58.9 (6)	C6—N4—C7—C8	57.6 (6)
C4—N1—C1—C2	56.9 (6)	N3—C8—C7—N4	−56.3 (6)
C3—N2—C2—C1	58.8 (6)	N4—C6—C5—N3	55.9 (5)
N1—C1—C2—N2	−56.7 (6)	C8—N3—C5—C6	−55.3 (5)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H9A···Cl2ⁱ	0.84 (4)	2.67 (6)	3.390 (7)	144 (6)
O1—H9B···Cl5ⁱⁱ	0.85 (6)	2.39 (6)	3.201 (6)	162 (5)
N1—H1A···Cl4ⁱⁱⁱ	0.90	2.40	3.181 (5)	145
N1—H1D···Cl4	0.90	2.57	3.284 (5)	137
N1—H1D···Cl5	0.90	2.75	3.455 (5)	136
N2—H2A···O1	0.90	1.82	2.705 (7)	167
N2—H2D···Cl7^iv	0.90	2.26	3.149 (5)	169
N3—H3C···Cl6	0.90	2.36	3.208 (5)	158
N3—H3D···Cl7^v	0.90	2.21	3.069 (5)	159
N4—H4C···Cl1^vi	0.90	2.37	3.228 (5)	158
N4—H4D···Cl4^vii	0.90	2.43	3.155 (5)	138

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H9A⋯Cl2ⁱ	0.84 (4)	2.67 (6)	3.390 (7)	144 (6)
O1—H9B⋯Cl5ⁱⁱ	0.85 (6)	2.39 (6)	3.201 (6)	162 (5)
N1—H1A⋯Cl4ⁱⁱⁱ	0.90	2.40	3.181 (5)	145
N1—H1D⋯Cl4	0.90	2.57	3.284 (5)	137
N1—H1D⋯Cl5	0.90	2.75	3.455 (5)	136
N2—H2A⋯O1	0.90	1.82	2.705 (7)	167
N2—H2D⋯Cl7^iv	0.90	2.26	3.149 (5)	169
N3—H3C⋯Cl6	0.90	2.36	3.208 (5)	158
N3—H3D⋯Cl7^v	0.90	2.21	3.069 (5)	159
N4—H4C⋯Cl1^vi	0.90	2.37	3.228 (5)	158
N4—H4D⋯Cl4^vii	0.90	2.43	3.155 (5)	138

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .

1 in total

1. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

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