catena-Poly[benzyl­trimethyl­ammonium [cadmium(II)-tri-μ2-thio­cyanato]]

Bala, R.; Kennedy, A.R.; Saneja, K.; Sharma, R.P.

doi:10.1107/S1600536806022938

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 62| Part 7| July 2006| Pages m1630-m1632

https://doi.org/10.1107/S1600536806022938

catena-Poly[benzyltrimethylammonium [cadmium(II)-tri-μ₂-thiocyanato]]

Ritu Bala,^a Alan R. Kennedy,^b Kalpna Saneja ^a and Raj Pal Sharma ^a ^*

^aChemistry Department, Panjab University, Chandigarh 160 014, India, and ^bWestCHEM, Department of Pure & Applied Chemistry, University of Strathclyde, 295 Cathedral Street, Glasgow G1 1XL, Scotland
^*Correspondence e-mail: rpsharmapu@yahoo.co.in

(Received 1 June 2006; accepted 14 June 2006; online 23 June 2006)

The title compound, {(C₁₀H₁₆N)[Cd(SCN)₃]}_n, contains [(C₆H₅CH₂)N(CH₃)₃]⁺ cations lying between one-dimensional chains of stoichiometry {[Cd(SCN)₃]⁻}_n. Each Cd^II ion is 3N,3S-hexacoordinated by thiocyanate ligands, in an octahedral fac arrangement. The asymmetric unit contains two cations and two anions.

Comment

In recent years, studies of the synthesis and properties of semiconductor materials such as CdS and CdSe have become an area of interest owing to the great scope for fundamental understanding of materials as well as potential technological applications (Zhang et al., 1999 ), such as light-emitting devices, non-linear optical devices, solar cells and biological labels. As a result, the search for new precursors, such as salts containing [Cd(SCN)₃]⁻, is receiving much attention. As the d¹⁰ configuration and softness of Cd^II permit a wide variety of geometries and coordination numbers, especially with the ambidentate ligand thiocyanate (SCN⁻), various structural types have been observed. Which structural type occurs depends on the size, shape and symmetry of the counter-cations and also on the ratio of Cd²⁺ to SCN⁻ ions. Thus, the structures of a number of one-dimensional single chains (Zhang et al., 2001 ), two-dimensional networks (Zhang et al., 1997 ) and three-dimensional structures (Thiele & Messer, 1980 ) have been reported and reviewed (Sun et al., 2001 ). Of special interest are the low-dimensional structural motifs, since these relate to highly anisotropic physical properties. In continuation of our interest in the supramolecular chemistry of salts of simple metal complexes (Sharma et al., 2005 , 2006 ), the synthesis and characterization of the title compound, (I), was undertaken.

For (I), structure determination revealed the presence of four crystallographically independent components in the solid state: two [(C₆H₅CH₂)N(CH₃)₃]⁺ cations and two [Cd(SCN)₃]⁻ anions (Fig. 1). Each Cd^II ion is 3N,3S-hexacoordinated, and adopts a slightly deformed fac octahedral geometry. Thus, each S atom is trans to an N atom. One of the thiocyanate ions (S6/C6/N6) appears to be rotationally disordered about its central C atom, which modifies the Cd^II coordination geometry at 9% of the Cd2 metal sites. Both the Cd—S and Cd—N bond lengths show considerable variation (Table 1). Similar distances (Cd—S = 2.688–2.743 Å and Cd—N = 2.279–2.379 Å) are observed in [(CH₃)₄N][Cd(SCN)₃], which is also 3N,3S-coordinated (Kuniyasu et al., 1987 ). The average Cd—N—C and Cd—S—C angles in (I) (142.11 and 98.93°, respectively) are also comparable with those in [(CH₃)₄N][Cd(SCN)₃]. The {[Cd(SCN)₃]⁻}_n chains (Fig. 2) propagate along the b-axis direction, with [Cd(SCN)₆] octahedra linked in a face-sharing manner via the shared SCN⁻ ligands. The [(C₆H₅CH₂)N(CH₃)₃]⁺ cations occupy positions between the chains. It is generally believed that the relative arrangement of the anionic {[Cd(SCN)₃]⁻}_n chains is strongly influenced by the size and shape of the cation. With larger cations, parallel alignment of the {[Cd(SCN)₃]⁻}_n chains is expected; this is observed in (I).

Figure 1
The contents of the asymmetric unit of (I)

, with displacement ellipsoids drawn at the 50% probability level for non-H atoms. The minor disorder component is indicated by dashed bonds.

Figure 2
The polymeric {[Cd(SCN)₃]⁻}_n chains extending along the b-axis direction.

Experimental

Analytical grade reagents were used without any further purification. Benzyltrimethylammonium chloride (1.0 g, 0.005 mol) was dissolved in 10 ml water, while CdCl₂ (0.98 g, 0.004 mol) and ammonium thiocyanate (1.22 g, 0.016 mol) were dissolved in 20 ml water by mechanical stirring. The solutions were mixed and a curd-like white solid precipitated immediately. This was filtered off and dried in air. Crystals of (I) were obtained after redissolving the white solid in an acetone–water mixture (1:1) at room temperature. The salt decomposes at 393 K and is insoluble in organic solvents (C₂H₅OH, CCl₄ and CH₃Cl), but soluble in DMSO and hot water. IR (KBr, ν, cm⁻¹): 2116 (s), 2087 (s, SCN), 1660 (m), 1553 (m), 1081 (s), 1028 (s), 1002 (s). ¹H NMR (d₆-DMSO, 298 K): δ 7.2 (s, 5H, HAr), 4.2 (s, 2H, ArCH₂), 2.6 (s, 9H, CH₃). ¹³C NMR (d₆-DMSO, 298 K): δ 128–133 (Ar), 126 (SCN), 68 (ArC), 25 (CH₃).

Crystal data

(C₁₀H₁₆N)[Cd(SCN)₃]
M_r = 436.88
Monoclinic, P 2₁
a = 9.9668 (3) Å
b = 10.8210 (3) Å
c = 16.5299 (5) Å
β = 102.351 (2)°
V = 1741.50 (9) Å³
Z = 4
D_x = 1.666 Mg m⁻³
Mo Kα radiation
μ = 1.61 mm⁻¹
T = 123 (2) K
Needle, colourless
0.35 × 0.08 × 0.06 mm

Data collection

Nonius KappaCCD diffractometer
φ and ω scans
Absorption correction: multi-scan (SORTAV; Blessing, 1997 ) T_min = 0.880, T_max = 0.908
31141 measured reflections
7120 independent reflections
5777 reflections with I > 2σ(I)
R_int = 0.060
θ_max = 27.1°

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.041
wR(F²) = 0.067
S = 1.06
7120 reflections
394 parameters
H-atom parameters constrained
w = 1/[σ²(F_o²) + (0.0138P)² + 2.3495P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max = 0.001
Δρ_max = 0.92 e Å⁻³
Δρ_min = −0.57 e Å⁻³
Absolute structure: Flack (1983 ), 3074 Friedel pairs
Flack parameter: −0.04 (2)

Table 1
Selected geometric parameters (Å, °)

Cd1—N1ⁱ	2.293 (5)
Cd1—N3ⁱⁱ	2.320 (5)
Cd1—N2ⁱⁱ	2.369 (5)
Cd1—S3	2.6749 (15)
Cd1—S1	2.7231 (15)
Cd1—S2	2.7350 (15)
Cd2—N4ⁱⁱⁱ	2.294 (5)
Cd2—N5^iv	2.341 (5)
Cd2—N6^iv	2.361 (6)
Cd2—S5	2.6925 (15)
Cd2—S4	2.7097 (15)
Cd2—S6	2.762 (2)

C1—S1—Cd1	94.81 (18)
C2—S2—Cd1	99.67 (17)
C3—S3—Cd1	99.07 (18)
C4—S4—Cd2	95.24 (18)
C5—S5—Cd2	98.12 (18)
C1—N1—Cd1ⁱⁱ	155.1 (4)
C2—N2—Cd1ⁱ	144.8 (4)
C3—N3—Cd1ⁱ	146.7 (4)
C4—N4—Cd2^iv	155.3 (4)
C5—N5—Cd2ⁱⁱⁱ	149.3 (4)
C6—S6—Cd2	102.2 (2)
C6—N6—Cd2ⁱⁱⁱ	140.2 (6)
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z-1]$ ; (ii) $[-x+1, y-{\script{1\over 2}}, -z-1]$ ; (iii) $[-x+2, y-{\script{1\over 2}}, -z]$ ; (iv) $[-x+2, y+{\script{1\over 2}}, -z]$ .

One SCN⁻ ligand (S6/C6/N6) was modelled as disordered by a rotation about the C atom, giving two S and two N sites. The site occupancies of the two components were refined to 0.911 (7):0.089 (7). All H atoms were placed in geometrically idealized positions and refined using a riding model: C—H = 0.95 Å for CH, 0.99 Å for CH₂ and 0.98 Å for CH₃; U_iso(H) = 1.2U_eq(C) for CH and CH₂, and U_iso(H) = 1.5U_eq(C) for CH₃. We have noted that many crystals from the sample were twinned so that they appeared C-centred monoclinic.

Data collection: COLLECT (Hooft, 1988 ) and DENZO (Otwinowski & Minor, 1997 ); cell refinement: DENZO and COLLECT; data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536806022938/bi2019sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536806022938/bi2019Isup2.hkl

Computing details top

Data collection: COLLECT (Hooft, 1988) and DENZO (Otwinowski & Minor, 1997); cell refinement: DENZO and COLLECT; data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP (Johnson, 1976); software used to prepare material for publication: SHELXL97.

catena-Poly[benzyltrimethylammonium [cadmium(II)-tri-µ₂-thiocyanato]] top

Crystal data top

(C₁₀H₁₆N)[Cd(SCN)₃]	F(000) = 872
M_r = 436.88	D_x = 1.666 Mg m⁻³
Monoclinic, P2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 23608 reflections
a = 9.9668 (3) Å	θ = 1.0–27.1°
b = 10.8210 (3) Å	µ = 1.61 mm⁻¹
c = 16.5299 (5) Å	T = 123 K
β = 102.351 (2)°	Needle, colourless
V = 1741.50 (9) Å³	0.35 × 0.08 × 0.06 mm
Z = 4

Data collection top

Nonius KappaCCD diffractometer	7120 independent reflections
Radiation source: fine-focus sealed tube	5777 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
φ and ω scans	θ_max = 27.1°, θ_min = 1.3°
Absorption correction: multi-scan (SORTAV; Blessing, 1997)	h = −12→12
T_min = 0.880, T_max = 0.908	k = −13→13
31141 measured reflections	l = −21→21

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)] = 0.041	H-atom parameters constrained
wR(F²) = 0.067	w = 1/[σ²(F_o²) + (0.0138P)² + 2.3495P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.001
7120 reflections	Δρ_max = 0.92 e Å⁻³
394 parameters	Δρ_min = −0.57 e Å⁻³
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.04 (2)

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	Occ. (<1)
Cd1	0.54939 (4)	1.08483 (3)	−0.48099 (2)	0.02172 (11)
Cd2	1.04903 (4)	0.95438 (3)	0.00501 (2)	0.02304 (12)
S1	0.75935 (15)	0.93665 (14)	−0.40456 (10)	0.0332 (4)
S2	0.73753 (15)	1.21949 (14)	−0.54232 (10)	0.0324 (4)
S3	0.58885 (15)	1.21984 (14)	−0.34235 (9)	0.0289 (3)
S4	1.24706 (14)	1.09470 (15)	−0.03894 (10)	0.0347 (4)
S5	1.25651 (15)	0.81422 (14)	0.08814 (10)	0.0322 (4)
N1	0.6246 (5)	0.7116 (5)	−0.4534 (3)	0.0304 (12)
N2	0.6041 (4)	1.4486 (5)	−0.5656 (3)	0.0301 (11)
N3	0.4838 (5)	1.4480 (5)	−0.4084 (3)	0.0308 (11)
N4	1.1085 (5)	1.3203 (4)	−0.0389 (3)	0.0294 (11)
N5	1.1295 (4)	0.5817 (5)	0.0633 (3)	0.0282 (10)
N7	0.9758 (5)	1.5170 (4)	−0.3537 (3)	0.0278 (12)
N8	1.4800 (5)	1.3837 (5)	0.1731 (3)	0.0277 (12)
C1	0.6774 (5)	0.8053 (5)	−0.4350 (3)	0.0245 (13)
C2	0.6582 (5)	1.3533 (5)	−0.5551 (3)	0.0205 (12)
C3	0.5262 (5)	1.3537 (5)	−0.3828 (3)	0.0216 (12)
C4	1.1641 (6)	1.2271 (5)	−0.0387 (3)	0.0276 (13)
C5	1.1788 (5)	0.6776 (5)	0.0729 (3)	0.0231 (12)
C6	0.9806 (6)	0.6968 (6)	−0.1253 (3)	0.0275 (13)
C7	1.0872 (5)	1.4559 (6)	−0.2890 (3)	0.0269 (12)
H7A	1.1773	1.4901	−0.2937	0.032*
H7B	1.0724	1.4774	−0.2333	0.032*
C8	1.0916 (5)	1.3183 (5)	−0.2964 (3)	0.0246 (12)
C9	1.1779 (5)	1.2627 (6)	−0.3405 (4)	0.0342 (15)
H9	1.2359	1.3122	−0.3660	0.041*
C10	1.1805 (6)	1.1351 (6)	−0.3480 (4)	0.0431 (18)
H10	1.2400	1.0974	−0.3786	0.052*
C11	1.0970 (6)	1.0634 (6)	−0.3112 (4)	0.0429 (19)
H11	1.0968	0.9761	−0.3176	0.051*
C12	1.0144 (6)	1.1170 (6)	−0.2653 (4)	0.0394 (16)
H12	0.9588	1.0668	−0.2386	0.047*
C13	1.0112 (6)	1.2443 (5)	−0.2575 (4)	0.0334 (15)
H13	0.9536	1.2810	−0.2253	0.040*
C14	0.8361 (5)	1.4800 (5)	−0.3441 (4)	0.0417 (17)
H14A	0.7669	1.5279	−0.3826	0.063*
H14B	0.8272	1.4960	−0.2872	0.063*
H14C	0.8223	1.3917	−0.3564	0.063*
C15	0.9914 (7)	1.4849 (6)	−0.4392 (4)	0.0453 (18)
H15A	0.9195	1.5265	−0.4798	0.068*
H15B	0.9830	1.3953	−0.4471	0.068*
H15C	1.0818	1.5120	−0.4466	0.068*
C16	0.9914 (7)	1.6546 (6)	−0.3426 (4)	0.0325 (16)
H16A	0.9700	1.6785	−0.2896	0.049*
H16B	0.9283	1.6966	−0.3879	0.049*
H16C	1.0861	1.6784	−0.3432	0.049*
C17	1.6052 (5)	1.3104 (5)	0.2175 (3)	0.0304 (14)
H17A	1.6892	1.3514	0.2078	0.036*
H17B	1.6087	1.3125	0.2778	0.036*
C18	1.6058 (5)	1.1769 (5)	0.1900 (3)	0.0254 (13)
C19	1.6736 (6)	1.1449 (6)	0.1271 (4)	0.0298 (14)
H19	1.7156	1.2072	0.1004	0.036*
C20	1.6796 (6)	1.0236 (6)	0.1038 (4)	0.0283 (14)
H20	1.7275	1.0022	0.0619	0.034*
C21	1.6171 (6)	0.9331 (6)	0.1405 (3)	0.0302 (14)
H21	1.6222	0.8495	0.1239	0.036*
C22	1.5470 (6)	0.9625 (7)	0.2011 (3)	0.0315 (14)
H22	1.5010	0.8999	0.2250	0.038*
C23	1.5441 (5)	1.0826 (6)	0.2268 (3)	0.0307 (13)
H23	1.4993	1.1021	0.2705	0.037*
C24	1.3513 (6)	1.3350 (8)	0.1914 (5)	0.062 (2)
H24A	1.3357	1.2507	0.1698	0.093*
H24B	1.2743	1.3878	0.1652	0.093*
H24C	1.3584	1.3342	0.2515	0.093*
C25	1.4688 (7)	1.3821 (6)	0.0818 (4)	0.0435 (17)
H25A	1.3919	1.4346	0.0550	0.065*
H25B	1.4530	1.2973	0.0612	0.065*
H25C	1.5542	1.4135	0.0690	0.065*
C26	1.5050 (8)	1.5163 (6)	0.2024 (5)	0.057 (2)
H26A	1.5179	1.5193	0.2628	0.085*
H26B	1.4257	1.5672	0.1772	0.085*
H26C	1.5874	1.5481	0.1861	0.085*
S6	1.02410 (17)	0.83781 (15)	−0.14613 (13)	0.0269 (6)	0.911 (7)
N6	0.9539 (8)	0.5939 (6)	−0.1144 (4)	0.0315 (13)	0.911 (7)
S6A	0.890 (2)	0.586 (2)	−0.1443 (11)	0.020 (5)*	0.089 (7)
N6A	1.012 (6)	0.816 (6)	−0.106 (4)	0.026 (15)*	0.089 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0238 (3)	0.0129 (2)	0.0283 (2)	0.0003 (2)	0.00529 (18)	−0.00081 (19)
Cd2	0.0250 (3)	0.0116 (2)	0.0341 (2)	0.0008 (2)	0.00975 (19)	−0.00035 (19)
S1	0.0286 (8)	0.0151 (8)	0.0492 (10)	−0.0008 (7)	−0.0069 (7)	0.0002 (7)
S2	0.0312 (8)	0.0200 (8)	0.0515 (10)	0.0061 (7)	0.0211 (8)	0.0064 (7)
S3	0.0395 (8)	0.0176 (8)	0.0287 (8)	−0.0013 (7)	0.0052 (7)	0.0011 (6)
S4	0.0292 (8)	0.0170 (8)	0.0629 (10)	0.0011 (8)	0.0215 (7)	−0.0004 (8)
S5	0.0293 (8)	0.0170 (8)	0.0449 (10)	−0.0048 (7)	−0.0043 (7)	0.0013 (7)
N1	0.031 (3)	0.015 (3)	0.037 (3)	0.002 (2)	−0.010 (2)	0.004 (2)
N2	0.027 (2)	0.021 (3)	0.046 (3)	0.000 (3)	0.015 (2)	0.010 (3)
N3	0.047 (3)	0.022 (3)	0.024 (3)	0.003 (3)	0.008 (2)	0.003 (3)
N4	0.036 (3)	0.012 (3)	0.045 (3)	−0.002 (2)	0.019 (2)	0.002 (2)
N5	0.025 (2)	0.012 (2)	0.048 (3)	−0.007 (2)	0.010 (2)	−0.006 (3)
N7	0.022 (3)	0.021 (3)	0.040 (3)	−0.002 (2)	0.004 (2)	0.002 (2)
N8	0.031 (3)	0.024 (3)	0.028 (3)	0.010 (2)	0.004 (2)	−0.001 (2)
C1	0.022 (3)	0.017 (3)	0.033 (3)	0.010 (3)	0.003 (2)	0.002 (3)
C2	0.019 (3)	0.025 (3)	0.021 (3)	−0.003 (3)	0.010 (2)	0.002 (2)
C3	0.026 (3)	0.022 (3)	0.017 (3)	−0.004 (3)	0.005 (2)	−0.004 (2)
C4	0.036 (3)	0.018 (3)	0.033 (3)	−0.012 (3)	0.016 (3)	0.001 (3)
C5	0.019 (3)	0.026 (3)	0.024 (3)	0.005 (3)	0.002 (2)	−0.002 (3)
C6	0.035 (3)	0.026 (4)	0.024 (3)	0.004 (3)	0.013 (3)	0.001 (3)
C7	0.021 (3)	0.028 (3)	0.029 (3)	−0.003 (3)	0.000 (2)	−0.007 (3)
C8	0.020 (3)	0.021 (3)	0.031 (3)	0.005 (3)	0.003 (2)	−0.005 (3)
C9	0.013 (3)	0.043 (4)	0.045 (4)	0.000 (3)	0.004 (3)	−0.011 (3)
C10	0.025 (4)	0.035 (4)	0.066 (5)	0.006 (3)	0.001 (3)	−0.023 (3)
C11	0.038 (4)	0.021 (4)	0.057 (5)	0.006 (3)	−0.018 (3)	−0.008 (3)
C12	0.042 (4)	0.025 (4)	0.045 (4)	0.001 (3)	−0.004 (3)	0.009 (3)
C13	0.039 (4)	0.029 (4)	0.030 (3)	0.008 (3)	0.001 (3)	0.002 (3)
C14	0.021 (3)	0.018 (4)	0.082 (5)	0.001 (3)	0.003 (3)	0.013 (3)
C15	0.074 (5)	0.029 (4)	0.029 (4)	−0.012 (3)	0.004 (3)	−0.010 (3)
C16	0.034 (4)	0.021 (4)	0.045 (4)	0.002 (3)	0.015 (3)	0.001 (3)
C17	0.025 (3)	0.036 (4)	0.027 (3)	0.007 (3)	0.000 (3)	−0.002 (3)
C18	0.022 (3)	0.026 (3)	0.026 (3)	0.000 (3)	0.000 (3)	−0.004 (3)
C19	0.025 (3)	0.033 (4)	0.032 (4)	−0.006 (3)	0.008 (3)	−0.001 (3)
C20	0.024 (3)	0.035 (4)	0.026 (3)	−0.002 (3)	0.008 (3)	−0.006 (3)
C21	0.037 (4)	0.020 (4)	0.030 (3)	0.001 (3)	−0.002 (3)	−0.004 (3)
C22	0.035 (4)	0.028 (4)	0.030 (3)	−0.007 (3)	0.004 (3)	0.001 (3)
C23	0.028 (3)	0.039 (4)	0.024 (3)	0.007 (3)	0.004 (2)	0.002 (3)
C24	0.032 (4)	0.070 (5)	0.092 (6)	0.015 (4)	0.033 (4)	0.018 (5)
C25	0.057 (4)	0.034 (4)	0.034 (4)	0.004 (3)	−0.002 (3)	0.003 (3)
C26	0.063 (5)	0.035 (4)	0.061 (5)	0.024 (4)	−0.010 (4)	−0.015 (4)
S6	0.0374 (10)	0.0153 (9)	0.0305 (13)	0.0010 (8)	0.0127 (8)	0.0029 (7)
N6	0.035 (4)	0.020 (3)	0.039 (3)	0.001 (3)	0.007 (3)	0.004 (3)

Geometric parameters (Å, º) top

Cd1—N1ⁱ	2.293 (5)	C8—C13	1.385 (8)
Cd1—N3ⁱⁱ	2.320 (5)	C9—C10	1.387 (8)
Cd1—N2ⁱⁱ	2.369 (5)	C9—H9	0.950
Cd1—S3	2.6749 (15)	C10—C11	1.373 (9)
Cd1—S1	2.7231 (15)	C10—H10	0.950
Cd1—S2	2.7350 (15)	C11—C12	1.362 (9)
Cd2—N4ⁱⁱⁱ	2.294 (5)	C11—H11	0.950
Cd2—N6A	2.34 (6)	C12—C13	1.385 (8)
Cd2—N5^iv	2.341 (5)	C12—H12	0.950
Cd2—N6^iv	2.361 (6)	C13—H13	0.950
Cd2—S6A^iv	2.664 (19)	C14—H14A	0.980
Cd2—S5	2.6925 (15)	C14—H14B	0.980
Cd2—S4	2.7097 (15)	C14—H14C	0.980
Cd2—S6	2.762 (2)	C15—H15A	0.980
S1—C1	1.663 (6)	C15—H15B	0.980
S2—C2	1.642 (6)	C15—H15C	0.980
S3—C3	1.661 (6)	C16—H16A	0.980
S4—C4	1.654 (6)	C16—H16B	0.980
S5—C5	1.663 (6)	C16—H16C	0.980
N1—C1	1.152 (7)	C17—C18	1.514 (8)
N1—Cd1ⁱⁱ	2.293 (5)	C17—H17A	0.990
N2—C2	1.159 (7)	C17—H17B	0.990
N2—Cd1ⁱ	2.369 (5)	C18—C23	1.396 (8)
N3—C3	1.150 (7)	C18—C19	1.400 (7)
N3—Cd1ⁱ	2.320 (5)	C19—C20	1.373 (7)
N4—C4	1.150 (7)	C19—H19	0.950
N4—Cd2^iv	2.294 (5)	C20—C21	1.369 (8)
N5—C5	1.145 (7)	C20—H20	0.950
N5—Cd2ⁱⁱⁱ	2.341 (5)	C21—C22	1.377 (7)
N7—C14	1.490 (7)	C21—H21	0.950
N7—C15	1.495 (7)	C22—C23	1.370 (9)
N7—C16	1.504 (7)	C22—H22	0.950
N7—C7	1.517 (7)	C23—H23	0.950
N8—C24	1.478 (8)	C24—H24A	0.980
N8—C25	1.489 (7)	C24—H24B	0.980
N8—C26	1.518 (8)	C24—H24C	0.980
N8—C17	1.527 (7)	C25—H25A	0.980
C6—N6	1.168 (8)	C25—H25B	0.980
C6—N6A	1.35 (6)	C25—H25C	0.980
C6—S6A	1.50 (2)	C26—H26A	0.980
C6—S6	1.642 (6)	C26—H26B	0.980
C7—C8	1.496 (8)	C26—H26C	0.980
C7—H7A	0.990	N6—Cd2ⁱⁱⁱ	2.361 (6)
C7—H7B	0.990	S6A—Cd2ⁱⁱⁱ	2.664 (19)
C8—C9	1.379 (7)

N1ⁱ—Cd1—N3ⁱⁱ	92.47 (17)	C13—C8—C7	120.5 (5)
N1ⁱ—Cd1—N2ⁱⁱ	92.87 (17)	C8—C9—C10	120.5 (6)
N3ⁱⁱ—Cd1—N2ⁱⁱ	82.29 (16)	C8—C9—H9	119.8
N1ⁱ—Cd1—S3	92.07 (12)	C10—C9—H9	119.8
N3ⁱⁱ—Cd1—S3	173.44 (13)	C11—C10—C9	119.9 (6)
N2ⁱⁱ—Cd1—S3	92.76 (12)	C11—C10—H10	120.1
N1ⁱ—Cd1—S1	178.92 (13)	C9—C10—H10	120.1
N3ⁱⁱ—Cd1—S1	87.47 (13)	C12—C11—C10	120.2 (6)
N2ⁱⁱ—Cd1—S1	88.19 (12)	C12—C11—H11	119.9
S3—Cd1—S1	88.08 (5)	C10—C11—H11	119.9
N1ⁱ—Cd1—S2	90.88 (13)	C11—C12—C13	120.3 (6)
N3ⁱⁱ—Cd1—S2	92.38 (12)	C11—C12—H12	119.9
N2ⁱⁱ—Cd1—S2	173.60 (12)	C13—C12—H12	119.9
S3—Cd1—S2	92.28 (5)	C12—C13—C8	120.3 (6)
S1—Cd1—S2	88.05 (5)	C12—C13—H13	119.8
N4ⁱⁱⁱ—Cd2—N6A	77.7 (18)	C8—C13—H13	119.8
N4ⁱⁱⁱ—Cd2—N5^iv	90.04 (16)	N7—C14—H14A	109.5
N6A—Cd2—N5^iv	91.2 (15)	N7—C14—H14B	109.5
N4ⁱⁱⁱ—Cd2—N6^iv	95.52 (18)	H14A—C14—H14B	109.5
N6A—Cd2—N6^iv	170.4 (14)	N7—C14—H14C	109.5
N5^iv—Cd2—N6^iv	82.0 (2)	H14A—C14—H14C	109.5
N4ⁱⁱⁱ—Cd2—S6A^iv	99.7 (4)	H14B—C14—H14C	109.5
N6A—Cd2—S6A^iv	171.9 (17)	N7—C15—H15A	109.5
N5^iv—Cd2—S6A^iv	96.5 (5)	N7—C15—H15B	109.5
N4ⁱⁱⁱ—Cd2—S5	90.59 (12)	H15A—C15—H15B	109.5
N6A—Cd2—S5	90.9 (15)	N7—C15—H15C	109.5
N5^iv—Cd2—S5	177.87 (13)	H15A—C15—H15C	109.5
N6^iv—Cd2—S5	95.9 (2)	H15B—C15—H15C	109.5
S6A^iv—Cd2—S5	81.4 (5)	N7—C16—H16A	109.5
N4ⁱⁱⁱ—Cd2—S4	174.82 (12)	N7—C16—H16B	109.5
N6A—Cd2—S4	98.5 (17)	H16A—C16—H16B	109.5
N5^iv—Cd2—S4	93.60 (12)	N7—C16—H16C	109.5
N6^iv—Cd2—S4	88.64 (15)	H16A—C16—H16C	109.5
S6A^iv—Cd2—S4	83.5 (4)	H16B—C16—H16C	109.5
S5—Cd2—S4	85.90 (5)	C18—C17—N8	114.0 (4)
N4ⁱⁱⁱ—Cd2—S6	89.88 (12)	C18—C17—H17A	108.8
N6A—Cd2—S6	13.5 (18)	N8—C17—H17A	108.8
N5^iv—Cd2—S6	85.43 (12)	C18—C17—H17B	108.8
N6^iv—Cd2—S6	166.3 (2)	N8—C17—H17B	108.8
S6A^iv—Cd2—S6	170.2 (4)	H17A—C17—H17B	107.7
S5—Cd2—S6	96.61 (5)	C23—C18—C19	118.1 (5)
S4—Cd2—S6	86.74 (5)	C23—C18—C17	122.4 (5)
C1—S1—Cd1	94.81 (18)	C19—C18—C17	119.5 (5)
C2—S2—Cd1	99.67 (17)	C20—C19—C18	120.1 (5)
C3—S3—Cd1	99.07 (18)	C20—C19—H19	119.9
C4—S4—Cd2	95.24 (18)	C18—C19—H19	119.9
C5—S5—Cd2	98.12 (18)	C21—C20—C19	120.6 (5)
C1—N1—Cd1ⁱⁱ	155.1 (4)	C21—C20—H20	119.7
C2—N2—Cd1ⁱ	144.8 (4)	C19—C20—H20	119.7
C3—N3—Cd1ⁱ	146.7 (4)	C20—C21—C22	120.5 (6)
C4—N4—Cd2^iv	155.3 (4)	C20—C21—H21	119.8
C5—N5—Cd2ⁱⁱⁱ	149.3 (4)	C22—C21—H21	119.8
C14—N7—C15	109.0 (5)	C23—C22—C21	119.5 (6)
C14—N7—C16	109.2 (5)	C23—C22—H22	120.2
C15—N7—C16	108.4 (5)	C21—C22—H22	120.2
C14—N7—C7	111.6 (4)	C22—C23—C18	121.2 (5)
C15—N7—C7	110.9 (4)	C22—C23—H23	119.4
C16—N7—C7	107.7 (5)	C18—C23—H23	119.4
C24—N8—C25	108.9 (5)	N8—C24—H24A	109.5
C24—N8—C26	111.2 (6)	N8—C24—H24B	109.5
C25—N8—C26	107.8 (5)	H24A—C24—H24B	109.5
C24—N8—C17	111.8 (5)	N8—C24—H24C	109.5
C25—N8—C17	111.0 (5)	H24A—C24—H24C	109.5
C26—N8—C17	106.0 (5)	H24B—C24—H24C	109.5
N1—C1—S1	177.0 (5)	N8—C25—H25A	109.5
N2—C2—S2	178.2 (5)	N8—C25—H25B	109.5
N3—C3—S3	177.9 (5)	H25A—C25—H25B	109.5
N4—C4—S4	178.7 (5)	N8—C25—H25C	109.5
N5—C5—S5	177.7 (5)	H25A—C25—H25C	109.5
N6—C6—N6A	158 (3)	H25B—C25—H25C	109.5
N6A—C6—S6A	156 (3)	N8—C26—H26A	109.5
N6—C6—S6	175.6 (5)	N8—C26—H26B	109.5
S6A—C6—S6	151.2 (8)	H26A—C26—H26B	109.5
C8—C7—N7	114.0 (4)	N8—C26—H26C	109.5
C8—C7—H7A	108.8	H26A—C26—H26C	109.5
N7—C7—H7A	108.8	H26B—C26—H26C	109.5
C8—C7—H7B	108.8	C6—S6—Cd2	102.2 (2)
N7—C7—H7B	108.8	C6—N6—Cd2ⁱⁱⁱ	140.2 (6)
H7A—C7—H7B	107.7	C6—S6A—Cd2ⁱⁱⁱ	103.4 (10)
C9—C8—C13	118.8 (5)	C6—N6A—Cd2	142 (5)
C9—C8—C7	120.7 (5)

N3ⁱⁱ—Cd1—S1—C1	−40.4 (2)	C7—C8—C9—C10	−179.2 (5)
N2ⁱⁱ—Cd1—S1—C1	42.0 (2)	C8—C9—C10—C11	−0.1 (10)
S3—Cd1—S1—C1	134.8 (2)	C9—C10—C11—C12	−1.9 (9)
S2—Cd1—S1—C1	−132.8 (2)	C10—C11—C12—C13	1.8 (9)
N1ⁱ—Cd1—S2—C2	26.0 (2)	C11—C12—C13—C8	0.2 (9)
N3ⁱⁱ—Cd1—S2—C2	118.5 (2)	C9—C8—C13—C12	−2.1 (8)
S3—Cd1—S2—C2	−66.1 (2)	C7—C8—C13—C12	179.2 (5)
S1—Cd1—S2—C2	−154.1 (2)	C24—N8—C17—C18	64.1 (7)
N1ⁱ—Cd1—S3—C3	−24.4 (2)	C25—N8—C17—C18	−57.7 (6)
N2ⁱⁱ—Cd1—S3—C3	−117.4 (2)	C26—N8—C17—C18	−174.6 (6)
N5^iv—Cd2—S4—C4	32.0 (2)	N8—C17—C18—C23	−88.5 (6)
N6^iv—Cd2—S4—C4	−49.9 (3)	N8—C17—C18—C19	93.3 (6)
S6A^iv—Cd2—S4—C4	−64.1 (5)	C23—C18—C19—C20	−0.8 (8)
S5—Cd2—S4—C4	−145.9 (2)	C17—C18—C19—C20	177.4 (5)
S6—Cd2—S4—C4	117.2 (2)	C18—C19—C20—C21	1.4 (9)
N4ⁱⁱⁱ—Cd2—S5—C5	31.1 (2)	C19—C20—C21—C22	0.1 (9)
N6A—Cd2—S5—C5	−46.6 (18)	C20—C21—C22—C23	−2.3 (8)
N6^iv—Cd2—S5—C5	126.7 (2)	C21—C22—C23—C18	2.9 (8)
S6A^iv—Cd2—S5—C5	130.8 (4)	C19—C18—C23—C22	−1.4 (8)
C14—N7—C7—C8	64.7 (6)	C17—C18—C23—C22	−179.5 (5)
C15—N7—C7—C8	−57.1 (6)	N4ⁱⁱⁱ—Cd2—S6—C6	−27.9 (2)
C16—N7—C7—C8	−175.6 (5)	N5^iv—Cd2—S6—C6	−118.0 (2)
N7—C7—C8—C9	94.0 (6)	N6^iv—Cd2—S6—C6	−141.3 (7)
N7—C7—C8—C13	−87.4 (6)	S5—Cd2—S6—C6	62.6 (2)
C13—C8—C9—C10	2.1 (8)	S4—Cd2—S6—C6	148.1 (2)

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

Acknowledgements

RB thanks the CSIR, New Delhi, India, for providing financial support for this work.

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Volume 62| Part 7| July 2006| Pages m1630-m1632

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