Bis[4-(dimethyl­amino)pyridinium] tetra­bromidocadmate(II) monohydrate

Lo, K.M.; Ng, S.W.

doi:10.1107/S1600536809014366

metal-organic compounds

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Volume 65| Part 5| May 2009| Page m560

doi:10.1107/S1600536809014366

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Bis[4-(dimethylamino)pyridinium] tetrabromidocadmate(II) monohydrate

Kong Mun Lo ^a and Seik Weng Ng ^a ^*

^aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: seikweng@um.edu.my

(Received 13 April 2009; accepted 17 April 2009; online 25 April 2009)

The Cd atom in the hydrated title salt, (C₇H₁₁N₂)₂[CdBr₄]·H₂O, exists in an approximately tetrahedral coordination geometry, with Br—Cd—Br angles in the range 105.52 (3)–111.50 (3)°. The cation, anion and water molecule interact by O—H⋯Br, N—H⋯Br and N—H⋯O hydrogen bonds, forming a linear chain structure running along the a axis.

Related literature

For other tetrahedral ammonium tetrabromidocadmates, see: Altermatt et al. (1979 ); Battaglia et al. (1991 ); Casals et al. (1987 ); Geselle & Fuess (1994 ); Ishihara et al. (1998 ); Krishnan et al. (1991 ); Sato et al. (1986 ); Waskowska (1994 ).

Experimental

Crystal data

(C₇H₁₁N₂)₂[CdBr₄]·H₂O
M_r = 696.41
Triclinic, $[P \overline 1]$
a = 7.8918 (2) Å
b = 8.1197 (2) Å
c = 17.2719 (4) Å
α = 95.481 (1)°
β = 99.747 (1)°
γ = 96.489 (1)°
V = 1076.35 (5) Å³
Z = 2
Mo Kα radiation
μ = 8.45 mm⁻¹
T = 100 K
0.25 × 0.25 × 0.25 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.258, T_max = 0.431 (expected range = 0.072–0.121)
6014 measured reflections
3711 independent reflections
3255 reflections with I > 2σ(I)
R_int = 0.022

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.131
S = 1.07
3711 reflections
221 parameters
H-atom parameters constrained
Δρ_max = 1.53 e Å⁻³
Δρ_min = −1.65 e Å⁻³

Table 1
Selected bond angles (°)

Br1—Cd1—Br2	109.23 (3)
Br1—Cd1—Br3	109.83 (3)
Br4—Cd1—Br1	111.50 (3)
Br2—Cd1—Br3	105.52 (3)
Br2—Cd1—Br4	110.72 (3)
Br3—Cd1—Br4	109.87 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H11⋯Br1	0.84	2.83	3.351 (7)	122
O1—H12⋯Br3ⁱ	0.84	2.67	3.511 (7)	172
N1—H1⋯Br2	0.88	2.56	3.373 (7)	154
N3—H3⋯O1	0.88	2.36	3.011 (10)	131
Symmetry code: (i) x-1, y, z.

Data collection: APEX2 (Bruker, 2008 ); cell refinement: APEX2; data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001 ); software used to prepare material for publication: pubCIF (Westrip, 2009 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809014366/sj2619sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809014366/sj2619Isup2.hkl

checkCIF report

Related literature top

For other tetrahedral ammonium tetrabromidocadmates, see: Altermatt et al. (1979); Battaglia et al. (1991); Casals et al. (1987); Geselle & Fuess (1994); Ishihara et al. (1998); Krishnan et al. (1991); Sato et al. (1986); Waskowska (1994).

Experimental top

Cadmium chloride (0.5 g, 2 mmol) dissolved in water (10 ml) and 4-dimethylaminopyridine hydrobromide perbromide (0.8 g, 2 mmol) dissolved in ethanol (80 ml) were mixed and the mixture heated for 1 h. Slow evaporation of the filtrate gave colorless crystals.

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: APEX2 (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: pubCIF (Westrip, 2009).

Figures top

Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of (C₇H₁₁N₂)₂(CdBr₄).H₂O at the 70% probability level. H atoms are drawn as spheres of arbitrary radius.

Bis[4-(dimethylamino)pyridinium] tetrabromidocadmate(II) monohydrate top

Crystal data top

(C₇H₁₁N₂)₂[CdBr₄]·H₂O	Z = 2
M_r = 696.41	F(000) = 664
Triclinic, P1	D_x = 2.149 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.8918 (2) Å	Cell parameters from 3763 reflections
b = 8.1197 (2) Å	θ = 2.4–28.2°
c = 17.2719 (4) Å	µ = 8.45 mm⁻¹
α = 95.481 (1)°	T = 100 K
β = 99.747 (1)°	Irregular block, colourless
γ = 96.489 (1)°	0.25 × 0.25 × 0.25 mm
V = 1076.35 (5) Å³

Data collection top

Bruker SMART APEX diffractometer	3711 independent reflections
Radiation source: fine-focus sealed tube	3255 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.022
ω scans	θ_max = 25.0°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
T_min = 0.258, T_max = 0.431	k = −9→9
6014 measured reflections	l = −20→20

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.131	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0774P)² + 6.748P] where P = (F_o² + 2F_c²)/3
3711 reflections	(Δ/σ)_max = 0.001
221 parameters	Δρ_max = 1.53 e Å⁻³
0 restraints	Δρ_min = −1.65 e Å⁻³

Crystal data top

(C₇H₁₁N₂)₂[CdBr₄]·H₂O	γ = 96.489 (1)°
M_r = 696.41	V = 1076.35 (5) Å³
Triclinic, P1	Z = 2
a = 7.8918 (2) Å	Mo Kα radiation
b = 8.1197 (2) Å	µ = 8.45 mm⁻¹
c = 17.2719 (4) Å	T = 100 K
α = 95.481 (1)°	0.25 × 0.25 × 0.25 mm
β = 99.747 (1)°

Data collection top

Bruker SMART APEX diffractometer	3711 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3255 reflections with I > 2σ(I)
T_min = 0.258, T_max = 0.431	R_int = 0.022
6014 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.131	H-atom parameters constrained
S = 1.07	Δρ_max = 1.53 e Å⁻³
3711 reflections	Δρ_min = −1.65 e Å⁻³
221 parameters

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

	x	y	z	U_iso*/U_eq
Cd1	0.56389 (6)	0.31451 (6)	0.25658 (3)	0.01616 (17)
Br1	0.43625 (10)	0.44170 (10)	0.37244 (5)	0.0256 (2)
Br2	0.53082 (10)	0.50457 (9)	0.14316 (5)	0.0237 (2)
Br3	0.89498 (9)	0.31530 (10)	0.30001 (4)	0.0205 (2)
Br4	0.41821 (9)	0.01732 (9)	0.20678 (4)	0.0209 (2)
O1	0.1769 (9)	0.6316 (8)	0.2453 (4)	0.0438 (17)
H11	0.2666	0.5854	0.2431	0.066*
H12	0.1005	0.5627	0.2575	0.066*
N1	0.8619 (9)	0.3422 (9)	0.0770 (4)	0.0280 (16)
H1	0.7974	0.3812	0.1095	0.034*
N2	1.1657 (8)	0.1572 (8)	−0.0724 (4)	0.0187 (13)
N3	0.2927 (8)	0.8098 (8)	0.4100 (4)	0.0233 (14)
H3	0.3098	0.7253	0.3777	0.028*
N4	0.1981 (8)	1.1958 (7)	0.5626 (3)	0.0150 (12)
C1	0.3353 (10)	0.8102 (9)	0.4877 (5)	0.0210 (16)
H1A	0.3895	0.7197	0.5070	0.025*
C2	0.3061 (9)	0.9320 (9)	0.5412 (5)	0.0199 (16)
H2	0.3352	0.9246	0.5963	0.024*
C3	0.2300 (9)	1.0730 (9)	0.5130 (4)	0.0143 (14)
C4	0.1916 (9)	1.0680 (9)	0.4308 (5)	0.0179 (15)
H4	0.1414	1.1579	0.4089	0.022*
C5	0.2228 (9)	0.9411 (9)	0.3813 (4)	0.0197 (15)
H5	0.1955	0.9438	0.3258	0.024*
C6	0.2363 (11)	1.1943 (10)	0.6469 (5)	0.0258 (18)
H6A	0.1801	1.0901	0.6608	0.039*
H6B	0.1928	1.2893	0.6729	0.039*
H6C	0.3620	1.2025	0.6645	0.039*
C7	0.1264 (10)	1.3411 (9)	0.5317 (5)	0.0195 (15)
H7A	0.2057	1.3956	0.5012	0.029*
H7B	0.1122	1.4203	0.5759	0.029*
H7C	0.0134	1.3043	0.4975	0.029*
C8	1.0058 (10)	0.2831 (10)	0.1052 (5)	0.0249 (17)
H8	1.0381	0.2845	0.1608	0.030*
C9	1.1099 (10)	0.2201 (10)	0.0575 (4)	0.0199 (15)
H9	1.2124	0.1779	0.0800	0.024*
C10	1.0651 (9)	0.2175 (8)	−0.0254 (4)	0.0163 (15)
C11	0.9084 (10)	0.2811 (9)	−0.0549 (5)	0.0221 (17)
H11A	0.8709	0.2804	−0.1102	0.026*
C12	0.8130 (10)	0.3430 (9)	−0.0026 (5)	0.0245 (17)
H12A	0.7100	0.3877	−0.0220	0.029*
C13	1.3311 (10)	0.1038 (11)	−0.0401 (5)	0.0274 (18)
H13A	1.3938	0.1870	0.0031	0.041*
H13B	1.4006	0.0925	−0.0818	0.041*
H13C	1.3100	−0.0040	−0.0199	0.041*
C14	1.1133 (11)	0.1373 (10)	−0.1580 (4)	0.0242 (17)
H14A	1.1968	0.0788	−0.1822	0.036*
H14B	1.1100	0.2474	−0.1766	0.036*
H14C	0.9979	0.0723	−0.1728	0.036*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0151 (3)	0.0170 (3)	0.0153 (3)	0.0015 (2)	0.0019 (2)	−0.0014 (2)
Br1	0.0261 (4)	0.0246 (4)	0.0270 (5)	0.0027 (3)	0.0108 (3)	−0.0031 (3)
Br2	0.0229 (4)	0.0236 (4)	0.0244 (4)	0.0049 (3)	0.0000 (3)	0.0067 (3)
Br3	0.0158 (4)	0.0304 (4)	0.0148 (4)	0.0038 (3)	0.0021 (3)	0.0002 (3)
Br4	0.0239 (4)	0.0184 (4)	0.0187 (4)	−0.0008 (3)	0.0038 (3)	−0.0013 (3)
O1	0.049 (4)	0.037 (4)	0.044 (4)	0.010 (3)	0.004 (3)	0.000 (3)
N1	0.025 (4)	0.027 (4)	0.034 (4)	−0.001 (3)	0.019 (3)	−0.005 (3)
N2	0.020 (3)	0.026 (3)	0.011 (3)	0.002 (3)	0.004 (2)	0.007 (3)
N3	0.024 (3)	0.024 (3)	0.023 (4)	0.000 (3)	0.010 (3)	0.000 (3)
N4	0.019 (3)	0.017 (3)	0.009 (3)	0.003 (2)	0.001 (2)	0.004 (2)
C1	0.022 (4)	0.016 (4)	0.028 (4)	0.004 (3)	0.007 (3)	0.013 (3)
C2	0.016 (3)	0.019 (4)	0.024 (4)	−0.002 (3)	0.003 (3)	0.003 (3)
C3	0.012 (3)	0.017 (3)	0.013 (4)	−0.002 (3)	−0.001 (3)	0.012 (3)
C4	0.011 (3)	0.020 (4)	0.022 (4)	−0.001 (3)	0.002 (3)	0.003 (3)
C5	0.021 (4)	0.023 (4)	0.015 (4)	0.000 (3)	0.007 (3)	0.001 (3)
C6	0.031 (4)	0.027 (4)	0.017 (4)	−0.008 (3)	0.010 (3)	−0.006 (3)
C7	0.023 (4)	0.013 (3)	0.023 (4)	0.006 (3)	0.003 (3)	−0.001 (3)
C8	0.026 (4)	0.026 (4)	0.022 (4)	−0.002 (3)	0.009 (3)	−0.007 (3)
C9	0.022 (4)	0.025 (4)	0.012 (4)	0.000 (3)	0.005 (3)	−0.001 (3)
C10	0.019 (4)	0.011 (3)	0.016 (4)	−0.006 (3)	−0.004 (3)	0.008 (3)
C11	0.020 (4)	0.021 (4)	0.020 (4)	−0.010 (3)	−0.005 (3)	0.009 (3)
C12	0.020 (4)	0.015 (4)	0.037 (5)	0.000 (3)	0.003 (3)	0.005 (3)
C13	0.022 (4)	0.028 (4)	0.031 (5)	0.002 (3)	0.003 (3)	0.001 (4)
C14	0.031 (4)	0.028 (4)	0.012 (4)	0.001 (3)	0.003 (3)	0.001 (3)

Geometric parameters (Å, º) top

Cd1—Br1	2.5706 (9)	C4—C5	1.347 (11)
Cd1—Br2	2.6044 (9)	C4—H4	0.9500
Cd1—Br3	2.5926 (8)	C5—H5	0.9500
Cd1—Br4	2.5546 (8)	C6—H6A	0.9800
O1—H11	0.8418	C6—H6B	0.9800
O1—H12	0.8427	C6—H6C	0.9800
N1—C8	1.318 (11)	C7—H7A	0.9800
N1—C12	1.364 (11)	C7—H7B	0.9800
N1—H1	0.8800	C7—H7C	0.9800
N2—C10	1.326 (10)	C8—C9	1.364 (11)
N2—C14	1.455 (10)	C8—H8	0.9500
N2—C13	1.460 (10)	C9—C10	1.414 (10)
N3—C1	1.327 (10)	C9—H9	0.9500
N3—C5	1.352 (10)	C10—C11	1.427 (11)
N3—H3	0.8800	C11—C12	1.367 (12)
N4—C3	1.325 (10)	C11—H11A	0.9500
N4—C6	1.438 (10)	C12—H12A	0.9500
N4—C7	1.472 (9)	C13—H13A	0.9800
C1—C2	1.355 (11)	C13—H13B	0.9800
C1—H1A	0.9500	C13—H13C	0.9800
C2—C3	1.439 (10)	C14—H14A	0.9800
C2—H2	0.9500	C14—H14B	0.9800
C3—C4	1.396 (10)	C14—H14C	0.9800

Br1—Cd1—Br2	109.23 (3)	N4—C6—H6C	109.5
Br1—Cd1—Br3	109.83 (3)	H6A—C6—H6C	109.5
Br4—Cd1—Br1	111.50 (3)	H6B—C6—H6C	109.5
Br2—Cd1—Br3	105.52 (3)	N4—C7—H7A	109.5
Br2—Cd1—Br4	110.72 (3)	N4—C7—H7B	109.5
Br3—Cd1—Br4	109.87 (3)	H7A—C7—H7B	109.5
H11—O1—H12	108.9	N4—C7—H7C	109.5
C8—N1—C12	120.1 (7)	H7A—C7—H7C	109.5
C8—N1—H1	120.0	H7B—C7—H7C	109.5
C12—N1—H1	120.0	N1—C8—C9	122.4 (8)
C10—N2—C14	121.3 (6)	N1—C8—H8	118.8
C10—N2—C13	121.3 (6)	C9—C8—H8	118.8
C14—N2—C13	117.4 (6)	C8—C9—C10	119.8 (7)
C1—N3—C5	119.1 (7)	C8—C9—H9	120.1
C1—N3—H3	120.5	C10—C9—H9	120.1
C5—N3—H3	120.5	N2—C10—C9	120.4 (7)
C3—N4—C6	121.8 (6)	N2—C10—C11	122.7 (7)
C3—N4—C7	120.0 (6)	C9—C10—C11	116.9 (7)
C6—N4—C7	118.2 (6)	C12—C11—C10	119.1 (7)
N3—C1—C2	123.8 (7)	C12—C11—H11A	120.4
N3—C1—H1A	118.1	C10—C11—H11A	120.4
C2—C1—H1A	118.1	N1—C12—C11	121.6 (7)
C1—C2—C3	118.8 (7)	N1—C12—H12A	119.2
C1—C2—H2	120.6	C11—C12—H12A	119.2
C3—C2—H2	120.6	N2—C13—H13A	109.5
N4—C3—C4	123.6 (6)	N2—C13—H13B	109.5
N4—C3—C2	121.4 (6)	H13A—C13—H13B	109.5
C4—C3—C2	114.9 (7)	N2—C13—H13C	109.5
C5—C4—C3	122.9 (7)	H13A—C13—H13C	109.5
C5—C4—H4	118.6	H13B—C13—H13C	109.5
C3—C4—H4	118.6	N2—C14—H14A	109.5
C4—C5—N3	120.5 (7)	N2—C14—H14B	109.5
C4—C5—H5	119.8	H14A—C14—H14B	109.5
N3—C5—H5	119.8	N2—C14—H14C	109.5
N4—C6—H6A	109.5	H14A—C14—H14C	109.5
N4—C6—H6B	109.5	H14B—C14—H14C	109.5
H6A—C6—H6B	109.5

C5—N3—C1—C2	3.0 (11)	C12—N1—C8—C9	−0.5 (12)
N3—C1—C2—C3	−2.3 (11)	N1—C8—C9—C10	0.4 (12)
C6—N4—C3—C4	178.6 (7)	C14—N2—C10—C9	173.5 (7)
C7—N4—C3—C4	−3.1 (10)	C13—N2—C10—C9	−4.7 (10)
C6—N4—C3—C2	−0.5 (10)	C14—N2—C10—C11	−6.1 (10)
C7—N4—C3—C2	177.7 (6)	C13—N2—C10—C11	175.7 (7)
C1—C2—C3—N4	179.9 (7)	C8—C9—C10—N2	179.7 (7)
C1—C2—C3—C4	0.6 (10)	C8—C9—C10—C11	−0.7 (10)
N4—C3—C4—C5	−179.1 (7)	N2—C10—C11—C12	−179.2 (7)
C2—C3—C4—C5	0.1 (10)	C9—C10—C11—C12	1.2 (10)
C3—C4—C5—N3	0.6 (11)	C8—N1—C12—C11	1.1 (11)
C1—N3—C5—C4	−2.1 (11)	C10—C11—C12—N1	−1.4 (11)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···Br1	0.84	2.83	3.351 (7)	122
O1—H12···Br3ⁱ	0.84	2.67	3.511 (7)	172
N1—H1···Br2	0.88	2.56	3.373 (7)	154
N3—H3···O1	0.88	2.36	3.011 (10)	131

Symmetry code: (i) x−1, y, z.

Experimental details

Crystal data
Chemical formula	(C₇H₁₁N₂)₂[CdBr₄]·H₂O
M_r	696.41
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	7.8918 (2), 8.1197 (2), 17.2719 (4)
α, β, γ (°)	95.481 (1), 99.747 (1), 96.489 (1)
V (Å³)	1076.35 (5)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	8.45
Crystal size (mm)	0.25 × 0.25 × 0.25

Data collection
Diffractometer	Bruker SMART APEX diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.258, 0.431
No. of measured, independent and observed [I > 2σ(I)] reflections	6014, 3711, 3255
R_int	0.022
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.131, 1.07
No. of reflections	3711
No. of parameters	221
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.53, −1.65

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), pubCIF (Westrip, 2009).

Selected bond angles (º) top

Br1—Cd1—Br2	109.23 (3)	Br2—Cd1—Br3	105.52 (3)
Br1—Cd1—Br3	109.83 (3)	Br2—Cd1—Br4	110.72 (3)
Br4—Cd1—Br1	111.50 (3)	Br3—Cd1—Br4	109.87 (3)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···Br1	0.84	2.83	3.351 (7)	122
O1—H12···Br3ⁱ	0.84	2.67	3.511 (7)	172
N1—H1···Br2	0.88	2.56	3.373 (7)	154
N3—H3···O1	0.88	2.36	3.011 (10)	131

Symmetry code: (i) x−1, y, z.

Acknowledgements

The authors thank the University of Malaya (grant No. FS339/2008A) for supporting this study.

References

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