Diisonicotinium penta­chloridoanti­monate(III) monohydrate

Chen, L.-Z.

doi:10.1107/S1600536809019072

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 6| June 2009| Page m683

doi:10.1107/S1600536809019072

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Diisonicotinium pentachloridoantimonate(III) monohydrate

Li-Zhuang Chen ^a ^*

^aOrdered Matter Science Research Center, College of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096, People's Republic of China
^*Correspondence e-mail: clz1977@sina.com

(Received 8 May 2009; accepted 20 May 2009; online 23 May 2009)

In the title compound, (C₆H₆NO₂)₂[SbCl₅]·H₂O, the Sb^III atom exhibits a distorted square-pyramidal coordination geometry. The crystal structure is stabilized by intermolecular N—H⋯Cl, N—H⋯O, O—H⋯Cl and O—H⋯O hydrogen bonds, forming an extended three-dimensional network.

Related literature

For related structures, see: Bujak & Zaleski (1999 ); Feng et al. (2007 ); Shen-Tu et al. (2008 ).

Experimental

Crystal data

(C₆H₆NO₂)₂[SbCl₅]·H₂O
M_r = 565.25
Monoclinic, P 2₁ /c
a = 10.334 (2) Å
b = 8.7319 (17) Å
c = 23.615 (7) Å
β = 106.98 (3)°
V = 2038.0 (9) Å³
Z = 4
Mo Kα radiation
μ = 2.03 mm⁻¹
T = 291 K
0.25 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ) T_min = 0.61, T_max = 0.67
19258 measured reflections
4675 independent reflections
4071 reflections with I > 2σ(I)
R_int = 0.061

Refinement

R[F² > 2σ(F²)] = 0.057
wR(F²) = 0.085
S = 1.19
4675 reflections
227 parameters
H-atom parameters constrained
Δρ_max = 0.76 e Å⁻³
Δρ_min = −1.76 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1C⋯O1Wⁱ	0.85	1.67	2.520 (5)	175
N1—H1B⋯O4ⁱⁱ	0.86	2.45	3.031 (6)	126
O1W—H1WA⋯Cl3ⁱⁱⁱ	0.85	2.71	3.378 (7)	136
O1W—H1WB⋯Cl5ⁱⁱⁱ	0.85	2.54	3.241 (4)	140
O3—H3A⋯Cl5ⁱⁱ	0.85	2.19	3.034 (4)	175
N2—H2A⋯O2^iv	0.86	2.41	2.988 (5)	125
N2—H2A⋯Cl2^v	0.86	2.49	3.224 (4)	144
N1—H1B⋯Cl5	0.86	2.42	3.147 (4)	143
Symmetry codes: (i) x, y+1, z; (ii) -x, -y+1, -z; (iii) x+1, y, z; (iv) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (v) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

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: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809019072/rz2323sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809019072/rz2323Isup2.hkl

checkCIF report

Comment top

Recently, the crystal structure of some halogenoantimonate salts has been reported (Feng et al.,2007; Bujak & Zaleski, 1999; Shen-Tu et al. 2008). As a contribution to this field, the synthesis and crystal structure of the title compound is reported herein.

The asymmetric unit of the title compound (Fig. 1) contains two protonated isonicotinic acid cations, a pentachloridoantimonate anion and a water molecule. The antimony(III) ion is in a distorted square-pyramidal coordination geometry, with the Sb—Cl distances ranging from 2.3642 (12) to 2.9002 (14) Å. This range of values is in agreement with that observed in N-methylpiperazinediium pentachloridoantimonate(III) monohydrate (2.4110 (10)–2.9112 (11) Å; Shen-Tu et al., 2008) and slightly larger than that reported for bis(ethyldimethylammonium) pentachloroantimonate(III) (2.499 (4)–2.768 (4) Å; Bujak & Zaleski, 1999). The crystal structure is stabilized by intermolecular N—H···Cl, N—H···O, O—H···Cl and O—H···O hydrogen bonds (Table 1), forming an extended three-dimensional network (Fig. 2).

Related literature top

For related structures, see: Bujak & Zaleski (1999); Feng et al. (2007); Shen-Tu et al. (2008).

Experimental top

SbCl₃, isonicotinic acid and 20% aqueous HCl in a molar ratio of 1:1:3 were mixed and dissolved in water by heating to 373 K forming a clear solution. The reaction mixture was cooled slowly to room temperature, crystals of the title compound were formed, collected and washed with dilute aqueous HCl.

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: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. A view of the title compound with the atom-numbering scheme. Displacement ellipsoids were drawn at the 30% probability level.
	Fig. 2. The crystal packing of the title compound viewed approximately along the b axis. Hydrogen bonds are drawn as dashed lines.

Diisonicotinium pentachloridoantimonate(III) monohydrate top

Crystal data top

(C₆H₆NO₂)₂[SbCl₅]·H₂O	F(000) = 1104
M_r = 565.25	D_x = 1.842 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4071 reflections
a = 10.334 (2) Å	θ = 3.1–27.5°
b = 8.7319 (17) Å	µ = 2.03 mm⁻¹
c = 23.615 (7) Å	T = 291 K
β = 106.98 (3)°	Block, colourless
V = 2038.0 (9) Å³	0.25 × 0.20 × 0.20 mm
Z = 4

Data collection top

Rigaku SCXmini diffractometer	4675 independent reflections
Radiation source: fine-focus sealed tube	4071 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.061
Detector resolution: 13.6612 pixels mm^-1	θ_max = 27.5°, θ_min = 3.1°
ω scans	h = −13→12
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	k = −11→11
T_min = 0.61, T_max = 0.67	l = −30→30
19258 measured reflections

Refinement top

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)] = 0.057	H-atom parameters constrained
wR(F²) = 0.085	w = 1/[σ²(F_o²) + (0.0112P)² + 1.8681P] where P = (F_o² + 2F_c²)/3
S = 1.19	(Δ/σ)_max < 0.001
4675 reflections	Δρ_max = 0.76 e Å⁻³
227 parameters	Δρ_min = −1.76 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0094 (3)

Crystal data top

(C₆H₆NO₂)₂[SbCl₅]·H₂O	V = 2038.0 (9) Å³
M_r = 565.25	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.334 (2) Å	µ = 2.03 mm⁻¹
b = 8.7319 (17) Å	T = 291 K
c = 23.615 (7) Å	0.25 × 0.20 × 0.20 mm
β = 106.98 (3)°

Data collection top

Rigaku SCXmini diffractometer	4675 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	4071 reflections with I > 2σ(I)
T_min = 0.61, T_max = 0.67	R_int = 0.061
19258 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.057	0 restraints
wR(F²) = 0.085	H-atom parameters constrained
S = 1.19	Δρ_max = 0.76 e Å⁻³
4675 reflections	Δρ_min = −1.76 e Å⁻³
227 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
O1	0.7498 (3)	0.9688 (4)	0.04677 (14)	0.0569 (9)
H1C	0.8214	1.0222	0.0583	0.085*
O2	0.8222 (3)	0.8846 (4)	0.14010 (14)	0.0583 (10)
N1	0.4007 (4)	0.6022 (5)	0.0507 (2)	0.0561 (11)
H1B	0.3308	0.5436	0.0427	0.067*
C1	0.4199 (5)	0.6891 (5)	0.0081 (2)	0.0527 (13)
H1A	0.3586	0.6866	−0.0296	0.063*
C6	0.7409 (5)	0.8855 (5)	0.0914 (2)	0.0419 (11)
C2	0.5301 (5)	0.7820 (5)	0.01973 (19)	0.0425 (11)
H2B	0.5451	0.8430	−0.0100	0.051*
C5	0.4841 (6)	0.6009 (6)	0.1054 (2)	0.0586 (14)
H5A	0.4668	0.5372	0.1338	0.070*
C4	0.5956 (5)	0.6935 (6)	0.1197 (2)	0.0489 (12)
H4A	0.6541	0.6947	0.1580	0.059*
C3	0.6198 (4)	0.7850 (5)	0.07631 (18)	0.0376 (10)
Cl5	0.21814 (12)	0.35116 (14)	0.08488 (5)	0.0501 (3)
O1W	0.9650 (5)	0.1234 (6)	0.0754 (3)	0.195 (4)
H1WA	1.0285	0.0715	0.0984	0.292*
H1WB	0.9982	0.2007	0.0627	0.292*
Sb1	0.38449 (3)	0.14611 (3)	0.173118 (11)	0.03103 (11)
Cl1	0.51635 (14)	−0.04608 (16)	0.24298 (6)	0.0646 (4)
Cl3	0.18317 (14)	0.09286 (16)	0.21279 (7)	0.0642 (4)
Cl2	0.60393 (12)	0.19468 (15)	0.13735 (5)	0.0521 (3)
Cl4	0.30831 (13)	−0.04201 (14)	0.09880 (6)	0.0554 (3)
O3	−0.0419 (4)	0.6811 (4)	0.04218 (15)	0.0734 (12)
H3A	−0.0944	0.6770	0.0070	0.110*
O4	−0.1684 (4)	0.4904 (5)	0.05540 (16)	0.0797 (13)
N2	0.1577 (4)	0.5697 (5)	0.25122 (17)	0.0513 (11)
H2A	0.2057	0.5670	0.2877	0.062*
C12	−0.0780 (5)	0.5765 (6)	0.0741 (2)	0.0474 (12)
C9	0.0065 (4)	0.5778 (5)	0.13730 (19)	0.0388 (10)
C8	−0.0139 (5)	0.4684 (6)	0.1746 (2)	0.0497 (12)
H8A	−0.0816	0.3958	0.1610	0.060*
C11	0.1813 (5)	0.6798 (6)	0.2169 (2)	0.0565 (14)
H11A	0.2490	0.7516	0.2321	0.068*
C10	0.1047 (5)	0.6868 (5)	0.1585 (2)	0.0528 (13)
H10A	0.1190	0.7639	0.1339	0.063*
C7	0.0648 (5)	0.4649 (6)	0.2321 (2)	0.0533 (13)
H7A	0.0525	0.3886	0.2576	0.064*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O1	0.051 (2)	0.072 (3)	0.046 (2)	−0.0181 (18)	0.0115 (17)	0.0049 (18)
O2	0.052 (2)	0.071 (3)	0.0415 (19)	0.0017 (18)	−0.0026 (17)	−0.0019 (17)
N1	0.060 (3)	0.047 (3)	0.062 (3)	−0.012 (2)	0.019 (2)	−0.002 (2)
C1	0.058 (3)	0.051 (3)	0.044 (3)	−0.010 (3)	0.007 (3)	−0.004 (2)
C6	0.039 (3)	0.050 (3)	0.036 (2)	0.003 (2)	0.009 (2)	−0.006 (2)
C2	0.048 (3)	0.047 (3)	0.031 (2)	−0.007 (2)	0.009 (2)	0.000 (2)
C5	0.077 (4)	0.050 (3)	0.058 (3)	0.001 (3)	0.033 (3)	0.014 (3)
C4	0.055 (3)	0.058 (3)	0.036 (3)	0.006 (3)	0.016 (2)	0.007 (2)
C3	0.040 (3)	0.044 (3)	0.032 (2)	0.004 (2)	0.015 (2)	−0.002 (2)
Cl5	0.0542 (7)	0.0498 (7)	0.0434 (6)	0.0001 (6)	0.0096 (6)	0.0118 (6)
O1W	0.074 (4)	0.146 (5)	0.316 (9)	−0.059 (4)	−0.017 (5)	0.112 (6)
Sb1	0.03618 (18)	0.02999 (17)	0.02550 (15)	0.00013 (12)	0.00678 (12)	0.00076 (12)
Cl1	0.0674 (9)	0.0654 (9)	0.0561 (8)	0.0156 (7)	0.0105 (7)	0.0324 (7)
Cl3	0.0663 (9)	0.0638 (9)	0.0750 (10)	−0.0064 (7)	0.0401 (8)	−0.0022 (7)
Cl2	0.0472 (7)	0.0707 (9)	0.0378 (6)	0.0062 (6)	0.0115 (6)	0.0107 (6)
Cl4	0.0676 (9)	0.0479 (7)	0.0506 (7)	−0.0077 (6)	0.0169 (7)	−0.0207 (6)
O3	0.094 (3)	0.070 (3)	0.041 (2)	−0.026 (2)	−0.005 (2)	0.0129 (18)
O4	0.079 (3)	0.102 (3)	0.043 (2)	−0.046 (3)	−0.006 (2)	0.007 (2)
N2	0.053 (3)	0.058 (3)	0.034 (2)	0.012 (2)	−0.0022 (19)	−0.002 (2)
C12	0.051 (3)	0.049 (3)	0.037 (3)	−0.002 (2)	0.006 (2)	−0.002 (2)
C9	0.039 (3)	0.039 (3)	0.035 (2)	0.004 (2)	0.005 (2)	−0.005 (2)
C8	0.053 (3)	0.053 (3)	0.039 (3)	−0.008 (2)	0.008 (2)	−0.003 (2)
C11	0.049 (3)	0.049 (3)	0.057 (3)	−0.004 (2)	−0.006 (3)	−0.006 (3)
C10	0.055 (3)	0.046 (3)	0.050 (3)	−0.005 (2)	0.002 (3)	0.007 (2)
C7	0.060 (3)	0.057 (3)	0.039 (3)	−0.001 (3)	0.008 (3)	0.007 (2)

Geometric parameters (Å, º) top

O1—C6	1.306 (5)	Sb1—Cl1	2.4661 (13)
O1—H1C	0.8500	Sb1—Cl3	2.5613 (15)
O2—C6	1.210 (5)	Sb1—Cl2	2.6748 (14)
N1—C1	1.322 (6)	O3—C12	1.306 (6)
N1—C5	1.325 (6)	O3—H3A	0.8500
N1—H1B	0.8600	O4—C12	1.180 (5)
C1—C2	1.359 (6)	N2—C7	1.307 (6)
C1—H1A	0.9300	N2—C11	1.326 (6)
C6—C3	1.484 (6)	N2—H2A	0.8600
C2—C3	1.386 (6)	C12—C9	1.493 (6)
C2—H2B	0.9300	C9—C8	1.357 (6)
C5—C4	1.366 (7)	C9—C10	1.375 (6)
C5—H5A	0.9300	C8—C7	1.365 (6)
C4—C3	1.379 (6)	C8—H8A	0.9300
C4—H4A	0.9300	C11—C10	1.375 (6)
O1W—H1WA	0.8500	C11—H11A	0.9300
O1W—H1WB	0.8499	C10—H10A	0.9300
Sb1—Cl5	2.9002 (14)	C7—H7A	0.9300
Sb1—Cl4	2.3646 (12)

C6—O1—H1C	107.9	Cl4—Sb1—Cl3	90.89 (5)
C1—N1—C5	123.2 (5)	Cl1—Sb1—Cl3	88.91 (5)
C1—N1—H1B	118.4	Cl4—Sb1—Cl2	90.28 (5)
C5—N1—H1B	118.4	Cl1—Sb1—Cl2	88.01 (5)
N1—C1—C2	119.4 (5)	Cl3—Sb1—Cl2	176.73 (4)
N1—C1—H1A	120.3	C12—O3—H3A	109.1
C2—C1—H1A	120.3	C7—N2—C11	123.0 (4)
O2—C6—O1	125.3 (5)	C7—N2—H2A	118.5
O2—C6—C3	121.8 (4)	C11—N2—H2A	118.5
O1—C6—C3	112.8 (4)	O4—C12—O3	123.9 (5)
C1—C2—C3	119.4 (5)	O4—C12—C9	123.2 (5)
C1—C2—H2B	120.3	O3—C12—C9	112.9 (4)
C3—C2—H2B	120.3	C8—C9—C10	119.2 (4)
N1—C5—C4	119.9 (5)	C8—C9—C12	119.2 (4)
N1—C5—H5A	120.1	C10—C9—C12	121.6 (4)
C4—C5—H5A	120.1	C9—C8—C7	120.1 (5)
C5—C4—C3	118.7 (5)	C9—C8—H8A	119.9
C5—C4—H4A	120.6	C7—C8—H8A	119.9
C3—C4—H4A	120.6	N2—C11—C10	119.3 (5)
C4—C3—C2	119.3 (4)	N2—C11—H11A	120.3
C4—C3—C6	119.2 (4)	C10—C11—H11A	120.3
C2—C3—C6	121.5 (4)	C9—C10—C11	118.8 (5)
H1WA—O1W—H1WB	109.5	C9—C10—H10A	120.6
Cl5—Sb1—Cl1	175.24 (4)	C11—C10—H10A	120.6
Cl5—Sb1—Cl3	90.03 (4)	N2—C7—C8	119.4 (5)
Cl5—Sb1—Cl2	93.12 (4)	N2—C7—H7A	120.3
Cl5—Sb1—Cl4	84.06 (4)	C8—C7—H7A	120.3
Cl4—Sb1—Cl1	91.32 (6)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1C···O1Wⁱ	0.85	1.67	2.520 (5)	175
N1—H1B···O4ⁱⁱ	0.86	2.45	3.031 (6)	126
O1W—H1WA···Cl3ⁱⁱⁱ	0.85	2.71	3.378 (7)	136
O1W—H1WB···Cl5ⁱⁱⁱ	0.85	2.54	3.241 (4)	140
O3—H3A···Cl5ⁱⁱ	0.85	2.19	3.034 (4)	175
N2—H2A···O2^iv	0.86	2.41	2.988 (5)	125
N2—H2A···Cl2^v	0.86	2.49	3.224 (4)	144
N1—H1B···Cl5	0.86	2.42	3.147 (4)	143

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

Experimental details

Crystal data
Chemical formula	(C₆H₆NO₂)₂[SbCl₅]·H₂O
M_r	565.25
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	291
a, b, c (Å)	10.334 (2), 8.7319 (17), 23.615 (7)
β (°)	106.98 (3)
V (Å³)	2038.0 (9)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.03
Crystal size (mm)	0.25 × 0.20 × 0.20

Data collection
Diffractometer	Rigaku SCXmini diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2005)
T_min, T_max	0.61, 0.67
No. of measured, independent and observed [I > 2σ(I)] reflections	19258, 4675, 4071
R_int	0.061
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.057, 0.085, 1.19
No. of reflections	4675
No. of parameters	227
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.76, −1.76

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1C···O1Wⁱ	0.85	1.67	2.520 (5)	175.0
N1—H1B···O4ⁱⁱ	0.86	2.45	3.031 (6)	125.5
O1W—H1WA···Cl3ⁱⁱⁱ	0.85	2.71	3.378 (7)	136.0
O1W—H1WB···Cl5ⁱⁱⁱ	0.85	2.54	3.241 (4)	140.0
O3—H3A···Cl5ⁱⁱ	0.85	2.19	3.034 (4)	174.8
N2—H2A···O2^iv	0.86	2.41	2.988 (5)	125.0
N2—H2A···Cl2^v	0.86	2.49	3.224 (4)	143.5
N1—H1B···Cl5	0.86	2.42	3.147 (4)	142.8

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

References

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ISSN: 2056-9890

Volume 65| Part 6| June 2009| Page m683

doi:10.1107/S1600536809019072

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