Monoclinic modification of 1,1,3,3,5,5-hexa­methyl-cyclo-1,3,5-tris­tannathiane

Singh, N.; Kumar, A.; Molloy, K.C.; Kociok-Köhn, G.

doi:10.1107/S1600536807063829

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 1| January 2008| Page m115

https://doi.org/10.1107/S1600536807063829

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Monoclinic modification of 1,1,3,3,5,5-hexamethyl-cyclo-1,3,5-tristannathiane

Nanhai Singh,^a ^* Abhinav Kumar,^a Kieran C. Molloy ^b and G. Kociok-Köhn ^b

^aDepartment of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi 221005, India, and ^bSchool of Chemistry, University of Bath, Bath BA2 7AY, England
^*Correspondence e-mail: nsingh@bhu.ac.in

(Received 10 November 2007; accepted 27 November 2007; online 6 December 2007)

The asymmetric unit of the title compound, [Sn₃(CH₃)₆S₃], contains two molecules with twist-boat conformations. There are intermolecular S⋯H (2.929 Å), S⋯S (3.433 Å), S⋯C (3.465 Å) and C⋯H (2.898 Å) interactions in addition to prominent intermolecular Sn⋯S interactions of 3.692 and 3.769 Å.

Related literature

For related literature, see: Menzebach & Bleckmann (1975 ) (tetragonal form); Jacobsen & Krebs (1977 ) (monoclinic form); Farina et al. (2001 ) (tetragonal form); Spek (2003 ).

Experimental

Crystal data

[Sn₃(CH₃)₆S₃]
M_r = 542.45
Monoclinic, P 2₁ /n
a = 14.826 (1) Å
b = 12.814 (1) Å
c = 17.744 (1) Å
β = 108.706 (1)°
V = 3192.94 (4) Å³
Z = 8
Mo Kα radiation
μ = 5.01 mm⁻¹
T = 150 (2) K
0.25 × 0.25 × 0.20 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (SORTAV; Blessing 1995 ) T_min = 0.311, T_max = 0.361
78537 measured reflections
9326 independent reflections
8221 reflections with I > 2σ(I)
R_int = 0.046

Refinement

R[F² > 2σ(F²)] = 0.030
wR(F²) = 0.067
S = 1.15
9326 reflections
229 parameters
H-atom parameters constrained
Δρ_max = 0.93 e Å⁻³
Δρ_min = −1.69 e Å⁻³

Data collection: COLLECT (Nonius, 1997–2000 ); cell refinement: HKL and SCALEPACK (Otwinowski & Minor, 1997 ); data reduction: DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536807063829/sg2203sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807063829/sg2203Isup2.hkl

checkCIF report

Comment top

Tris(dimethyltin sulfide),1,1,3,3,5,5-hexamethyl-cyclo-1,3,5-tristannathiane was the unexpected product in our attempt to synthesizing dimethyltin(emda) (emda = 1-ethoxycarbonyl-1-methylcarbonyl-2,2-dithiolate) (see Experimental). The literature reports that the compound crystallizes in monoclinic (P2₁/c; Jacobsen & Krebs, 1977), tetragonal (P₄; Menzebach & Bleckmann,1975) and tetragonal (P4₂2₁2; Farina et al., 2001) modifications. The monoclinic modification was refined in the P2₁/c space group. However, the checking program PLATON (Spek, 2003) finds P2₁/n space group which is now being authenticated in the present study. In the monoclinic unit cell the molecules are linked by Sn···S interaction of 3.692 and 3.796 Å, S···H interaction of 2.929 Å, S···S interaction of 3.433 Å, S···C interaction of 3.465 Å and C···H interaction of 2.898 Å.

Related literature top

For related literature, see: Menzebach & Bleckmann (1975) (tetragonal form); Jacobsen & Krebs (1977) (monoclinic form); Farina et al. (2001) (tetragonal form); Spek (2003).

Experimental top

To a stirring 20 ml me thanolic solution of K₂emda(1 mmol) was added, 15 ml me thanolic solution of dimethyltin(IV) chloride (1 mmol). The mixture was additionally stirred for 2 h. Whole solvent was vacuum evaporated toobtain solid residue. To this 20 ml chloroform was added and suction filteredto discard KCl. The orange coloured solution thus obtained was layered with methanol to afford yellow crystals.

Structure description top

For related literature, see: Menzebach & Bleckmann (1975) (tetragonal form); Jacobsen & Krebs (1977) (monoclinic form); Farina et al. (2001) (tetragonal form); Spek (2003).

Computing details top

Data collection: Collect (Nonius, 1997-2000); cell refinement: HKL and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

Figures top

	Fig. 1. ORTEP plot of tris(dimethyltin sulfide) at the 30% probability level.
	Fig. 2. Unit cell packing of tris(dimethyltin sulfide) showing Sn···S, S···S, S···H, S···C and C···H interactions.

1,1,3,3,5,5-hexamethyl-cyclo-1,3,5-tristannathiane top

Crystal data top

[Sn₃(CH₃)₆S₃]	D_x = 2.257 Mg m⁻³
M_r = 542.45	Melting point: 148 K
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 14.826 (1) Å	Cell parameters from 24000 reflections
b = 12.814 (1) Å	θ = 2.9–27.5°
c = 17.744 (1) Å	µ = 5.01 mm⁻¹
β = 108.706 (1)°	T = 150 K
V = 3192.94 (4) Å³	Block, yellow
Z = 8	0.25 × 0.25 × 0.20 mm
F(000) = 2016

Data collection top

Nonius KappaCCD diffractometer	9326 independent reflections
Radiation source: fine-focus sealed tube	8221 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.046
363 1.6 degree images with φ andω scans	θ_max = 30.1°, θ_min = 3.2°
Absorption correction: multi-scan (SORTAV; Blessing 1995)	h = −19→20
T_min = 0.311, T_max = 0.361	k = −17→18
78537 measured reflections	l = −24→24

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)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.067	H-atom parameters constrained
S = 1.15	w = 1/[σ²(F_o²) + (0.0287P)² + 3.7599P] where P = (F_o² + 2F_c²)/3
9326 reflections	(Δ/σ)_max = 0.002
229 parameters	Δρ_max = 0.93 e Å⁻³
0 restraints	Δρ_min = −1.69 e Å⁻³

Crystal data top

[Sn₃(CH₃)₆S₃]	V = 3192.94 (4) Å³
M_r = 542.45	Z = 8
Monoclinic, P2₁/n	Mo Kα radiation
a = 14.826 (1) Å	µ = 5.01 mm⁻¹
b = 12.814 (1) Å	T = 150 K
c = 17.744 (1) Å	0.25 × 0.25 × 0.20 mm
β = 108.706 (1)°

Data collection top

Nonius KappaCCD diffractometer	9326 independent reflections
Absorption correction: multi-scan (SORTAV; Blessing 1995)	8221 reflections with I > 2σ(I)
T_min = 0.311, T_max = 0.361	R_int = 0.046
78537 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.030	0 restraints
wR(F²) = 0.067	H-atom parameters constrained
S = 1.15	Δρ_max = 0.93 e Å⁻³
9326 reflections	Δρ_min = −1.69 e Å⁻³
229 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
Sn1	0.407801 (14)	−0.393311 (15)	0.330468 (12)	0.02220 (5)
Sn2	0.292630 (16)	−0.244657 (15)	0.143631 (12)	0.02433 (5)
Sn3	0.260380 (14)	−0.539580 (15)	0.143724 (12)	0.02231 (5)
Sn4	0.595000 (14)	0.105237 (15)	0.215469 (13)	0.02279 (5)
Sn5	0.775307 (14)	0.255910 (15)	0.373674 (12)	0.02168 (5)
Sn6	0.784610 (16)	−0.045519 (16)	0.370081 (13)	0.02807 (5)
S1	0.38690 (6)	−0.21710 (6)	0.28053 (5)	0.02717 (15)
S2	0.34811 (6)	−0.40429 (6)	0.10117 (5)	0.02742 (16)
S3	0.26038 (5)	−0.48569 (6)	0.27553 (4)	0.02501 (14)
S4	0.73866 (6)	0.00869 (6)	0.23204 (5)	0.02779 (15)
S5	0.74693 (8)	0.10168 (6)	0.44061 (5)	0.03455 (19)
S6	0.63617 (6)	0.28120 (6)	0.25940 (5)	0.02786 (15)
C1	0.5255 (3)	−0.4688 (3)	0.3101 (3)	0.0405 (8)
H1A	0.5840	−0.4305	0.3374	0.061*
H1B	0.5160	−0.4705	0.2528	0.061*
H1C	0.5306	−0.5403	0.3306	0.061*
C2	0.4245 (3)	−0.3748 (3)	0.4546 (2)	0.0427 (9)
H2A	0.4120	−0.4415	0.4764	0.064*
H2B	0.3794	−0.3222	0.4609	0.064*
H2C	0.4896	−0.3522	0.4832	0.064*
C3	0.1441 (2)	−0.2544 (3)	0.1283 (2)	0.0361 (8)
H3A	0.1203	−0.1853	0.1360	0.054*
H3B	0.1340	−0.3032	0.1673	0.054*
H3C	0.1100	−0.2793	0.0744	0.054*
C4	0.3309 (3)	−0.1254 (3)	0.0757 (2)	0.0411 (9)
H4A	0.2846	−0.1239	0.0220	0.062*
H4B	0.3945	−0.1398	0.0724	0.062*
H4C	0.3313	−0.0577	0.1014	0.062*
C5	0.1159 (2)	−0.5364 (3)	0.06916 (19)	0.0285 (6)
H5A	0.0969	−0.6062	0.0472	0.043*
H5B	0.1090	−0.4869	0.0256	0.043*
H5C	0.0753	−0.5146	0.1003	0.043*
C6	0.3447 (2)	−0.6776 (2)	0.1555 (2)	0.0298 (6)
H6A	0.3090	−0.7375	0.1655	0.045*
H6B	0.4038	−0.6693	0.2000	0.045*
H6C	0.3598	−0.6892	0.1063	0.045*
C7	0.5300 (3)	0.1155 (3)	0.0895 (2)	0.0423 (9)
H7A	0.5087	0.0461	0.0680	0.063*
H7B	0.5763	0.1425	0.0655	0.063*
H7C	0.4751	0.1627	0.0774	0.063*
C8	0.5078 (3)	0.0398 (3)	0.2777 (3)	0.0429 (9)
H8A	0.4453	0.0737	0.2603	0.064*
H8B	0.5379	0.0506	0.3350	0.064*
H8C	0.5001	−0.0352	0.2665	0.064*
C9	0.7751 (3)	0.3803 (2)	0.4535 (2)	0.0313 (7)
H9A	0.7892	0.3526	0.5075	0.047*
H9B	0.7123	0.4138	0.4371	0.047*
H9C	0.8236	0.4318	0.4525	0.047*
C10	0.9028 (3)	0.2408 (3)	0.3437 (2)	0.0364 (8)
H10A	0.9176	0.3075	0.3233	0.055*
H10B	0.8942	0.1869	0.3027	0.055*
H10C	0.9554	0.2209	0.3912	0.055*
C11	0.6965 (3)	−0.1716 (3)	0.3834 (2)	0.0416 (9)
H11A	0.7122	−0.2347	0.3589	0.062*
H11B	0.6295	−0.1537	0.3573	0.062*
H11C	0.7075	−0.1843	0.4401	0.062*
C12	0.9340 (3)	−0.0702 (3)	0.4128 (2)	0.0425 (9)
H12A	0.9538	−0.0860	0.4698	0.064*
H12B	0.9667	−0.0072	0.4040	0.064*
H12C	0.9503	−0.1289	0.3842	0.064*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sn1	0.02077 (10)	0.02012 (10)	0.02404 (10)	0.00078 (7)	0.00487 (8)	0.00072 (7)
Sn2	0.02967 (11)	0.01939 (10)	0.02465 (10)	0.00053 (7)	0.00974 (8)	0.00356 (7)
Sn3	0.02227 (10)	0.01899 (9)	0.02482 (10)	0.00015 (7)	0.00638 (8)	−0.00101 (7)
Sn4	0.02074 (10)	0.02090 (10)	0.02697 (11)	−0.00286 (7)	0.00798 (8)	−0.00433 (7)
Sn5	0.02387 (10)	0.01951 (10)	0.02113 (10)	0.00017 (7)	0.00645 (8)	−0.00146 (7)
Sn6	0.03327 (12)	0.01932 (10)	0.02936 (11)	−0.00007 (8)	0.00690 (9)	0.00062 (8)
S1	0.0324 (4)	0.0176 (3)	0.0293 (4)	−0.0025 (3)	0.0070 (3)	−0.0022 (3)
S2	0.0326 (4)	0.0234 (4)	0.0311 (4)	−0.0020 (3)	0.0171 (3)	−0.0019 (3)
S3	0.0253 (3)	0.0250 (4)	0.0266 (3)	−0.0048 (3)	0.0110 (3)	−0.0019 (3)
S4	0.0304 (4)	0.0268 (4)	0.0287 (4)	0.0056 (3)	0.0129 (3)	−0.0016 (3)
S5	0.0580 (6)	0.0244 (4)	0.0275 (4)	0.0035 (3)	0.0225 (4)	0.0037 (3)
S6	0.0296 (4)	0.0178 (3)	0.0299 (4)	0.0010 (3)	0.0008 (3)	0.0002 (3)
C1	0.0286 (17)	0.040 (2)	0.054 (2)	0.0095 (15)	0.0137 (16)	0.0019 (17)
C2	0.053 (2)	0.048 (2)	0.0230 (16)	−0.0027 (18)	0.0071 (16)	−0.0010 (15)
C3	0.0268 (17)	0.0341 (18)	0.043 (2)	0.0044 (13)	0.0058 (15)	−0.0018 (14)
C4	0.064 (3)	0.0281 (17)	0.040 (2)	0.0004 (17)	0.0280 (19)	0.0102 (14)
C5	0.0243 (14)	0.0335 (16)	0.0260 (15)	0.0020 (12)	0.0056 (12)	0.0023 (12)
C6	0.0322 (16)	0.0234 (14)	0.0351 (16)	0.0051 (12)	0.0126 (13)	0.0015 (12)
C7	0.038 (2)	0.050 (2)	0.0300 (18)	0.0039 (16)	−0.0020 (15)	−0.0081 (15)
C8	0.0358 (19)	0.042 (2)	0.059 (2)	−0.0133 (16)	0.0270 (18)	−0.0004 (17)
C9	0.0403 (18)	0.0248 (15)	0.0263 (15)	0.0008 (13)	0.0071 (14)	−0.0085 (12)
C10	0.0282 (17)	0.0370 (18)	0.049 (2)	0.0013 (13)	0.0187 (15)	0.0021 (15)
C11	0.051 (2)	0.0274 (17)	0.041 (2)	−0.0122 (16)	0.0082 (17)	0.0065 (14)
C12	0.0344 (19)	0.046 (2)	0.039 (2)	0.0020 (16)	−0.0001 (15)	−0.0160 (17)

Geometric parameters (Å, º) top

Sn1—C1	2.125 (3)	C3—H3A	0.9800
Sn1—C2	2.149 (4)	C3—H3B	0.9800
Sn1—S3	2.4005 (8)	C3—H3C	0.9800
Sn1—S1	2.4090 (8)	C4—H4A	0.9800
Sn2—C4	2.133 (3)	C4—H4B	0.9800
Sn2—C3	2.133 (4)	C4—H4C	0.9800
Sn2—S1	2.4086 (8)	C5—H5A	0.9800
Sn2—S2	2.4136 (8)	C5—H5B	0.9800
Sn3—C5	2.126 (3)	C5—H5C	0.9800
Sn3—C6	2.136 (3)	C6—H6A	0.9800
Sn3—S2	2.4284 (8)	C6—H6B	0.9800
Sn3—S3	2.4386 (8)	C6—H6C	0.9800
Sn4—C8	2.123 (3)	C7—H7A	0.9800
Sn4—C7	2.135 (4)	C7—H7B	0.9800
Sn4—S4	2.3982 (8)	C7—H7C	0.9800
Sn4—S6	2.3999 (8)	C8—H8A	0.9800
Sn5—C10	2.131 (3)	C8—H8B	0.9800
Sn5—C9	2.133 (3)	C8—H8C	0.9800
Sn5—S6	2.4060 (8)	C9—H9A	0.9800
Sn5—S5	2.4112 (8)	C9—H9B	0.9800
Sn6—C12	2.121 (4)	C9—H9C	0.9800
Sn6—C11	2.138 (3)	C10—H10A	0.9800
Sn6—S4	2.4240 (8)	C10—H10B	0.9800
Sn6—S5	2.4259 (8)	C10—H10C	0.9800
C1—H1A	0.9800	C11—H11A	0.9800
C1—H1B	0.9800	C11—H11B	0.9800
C1—H1C	0.9800	C11—H11C	0.9800
C2—H2A	0.9800	C12—H12A	0.9800
C2—H2B	0.9800	C12—H12B	0.9800
C2—H2C	0.9800	C12—H12C	0.9800

C1—Sn1—C2	113.19 (17)	Sn2—C3—H3C	109.5
C1—Sn1—S3	113.37 (11)	H3A—C3—H3C	109.5
C2—Sn1—S3	105.13 (12)	H3B—C3—H3C	109.5
C1—Sn1—S1	112.33 (11)	Sn2—C4—H4A	109.5
C2—Sn1—S1	103.44 (12)	Sn2—C4—H4B	109.5
S3—Sn1—S1	108.66 (3)	H4A—C4—H4B	109.5
C4—Sn2—C3	114.88 (16)	Sn2—C4—H4C	109.5
C4—Sn2—S1	106.94 (12)	H4A—C4—H4C	109.5
C3—Sn2—S1	112.25 (11)	H4B—C4—H4C	109.5
C4—Sn2—S2	104.57 (11)	Sn3—C5—H5A	109.5
C3—Sn2—S2	110.58 (10)	Sn3—C5—H5B	109.5
S1—Sn2—S2	107.06 (3)	H5A—C5—H5B	109.5
C5—Sn3—C6	121.18 (13)	Sn3—C5—H5C	109.5
C5—Sn3—S2	109.01 (9)	H5A—C5—H5C	109.5
C6—Sn3—S2	105.44 (9)	H5B—C5—H5C	109.5
C5—Sn3—S3	106.35 (9)	Sn3—C6—H6A	109.5
C6—Sn3—S3	108.70 (9)	Sn3—C6—H6B	109.5
S2—Sn3—S3	105.12 (3)	H6A—C6—H6B	109.5
C8—Sn4—C7	115.01 (17)	Sn3—C6—H6C	109.5
C8—Sn4—S4	113.41 (12)	H6A—C6—H6C	109.5
C7—Sn4—S4	104.21 (11)	H6B—C6—H6C	109.5
C8—Sn4—S6	109.64 (11)	Sn4—C7—H7A	109.5
C7—Sn4—S6	105.33 (11)	Sn4—C7—H7B	109.5
S4—Sn4—S6	108.75 (3)	H7A—C7—H7B	109.5
C10—Sn5—C9	115.11 (15)	Sn4—C7—H7C	109.5
C10—Sn5—S6	113.04 (11)	H7A—C7—H7C	109.5
C9—Sn5—S6	105.97 (10)	H7B—C7—H7C	109.5
C10—Sn5—S5	110.93 (10)	Sn4—C8—H8A	109.5
C9—Sn5—S5	104.36 (10)	Sn4—C8—H8B	109.5
S6—Sn5—S5	106.72 (3)	H8A—C8—H8B	109.5
C12—Sn6—C11	116.90 (17)	Sn4—C8—H8C	109.5
C12—Sn6—S4	109.05 (12)	H8A—C8—H8C	109.5
C11—Sn6—S4	110.17 (11)	H8B—C8—H8C	109.5
C12—Sn6—S5	108.57 (10)	Sn5—C9—H9A	109.5
C11—Sn6—S5	106.29 (12)	Sn5—C9—H9B	109.5
S4—Sn6—S5	105.18 (3)	H9A—C9—H9B	109.5
Sn2—S1—Sn1	101.43 (3)	Sn5—C9—H9C	109.5
Sn2—S2—Sn3	103.76 (3)	H9A—C9—H9C	109.5
Sn1—S3—Sn3	104.42 (3)	H9B—C9—H9C	109.5
Sn4—S4—Sn6	102.86 (3)	Sn5—C10—H10A	109.5
Sn5—S5—Sn6	106.13 (3)	Sn5—C10—H10B	109.5
Sn4—S6—Sn5	101.96 (3)	H10A—C10—H10B	109.5
Sn1—C1—H1A	109.5	Sn5—C10—H10C	109.5
Sn1—C1—H1B	109.5	H10A—C10—H10C	109.5
H1A—C1—H1B	109.5	H10B—C10—H10C	109.5
Sn1—C1—H1C	109.5	Sn6—C11—H11A	109.5
H1A—C1—H1C	109.5	Sn6—C11—H11B	109.5
H1B—C1—H1C	109.5	H11A—C11—H11B	109.5
Sn1—C2—H2A	109.5	Sn6—C11—H11C	109.5
Sn1—C2—H2B	109.5	H11A—C11—H11C	109.5
H2A—C2—H2B	109.5	H11B—C11—H11C	109.5
Sn1—C2—H2C	109.5	Sn6—C12—H12A	109.5
H2A—C2—H2C	109.5	Sn6—C12—H12B	109.5
H2B—C2—H2C	109.5	H12A—C12—H12B	109.5
Sn2—C3—H3A	109.5	Sn6—C12—H12C	109.5
Sn2—C3—H3B	109.5	H12A—C12—H12C	109.5
H3A—C3—H3B	109.5	H12B—C12—H12C	109.5

Experimental details

Crystal data
Chemical formula	[Sn₃(CH₃)₆S₃]
M_r	542.45
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	150
a, b, c (Å)	14.826 (1), 12.814 (1), 17.744 (1)
β (°)	108.706 (1)
V (Å³)	3192.94 (4)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	5.01
Crystal size (mm)	0.25 × 0.25 × 0.20

Data collection
Diffractometer	Nonius KappaCCD
Absorption correction	Multi-scan (SORTAV; Blessing 1995)
T_min, T_max	0.311, 0.361
No. of measured, independent and observed [I > 2σ(I)] reflections	78537, 9326, 8221
R_int	0.046
(sin θ/λ)_max (Å⁻¹)	0.705

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.030, 0.067, 1.15
No. of reflections	9326
No. of parameters	229
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.93, −1.69

Computer programs: Collect (Nonius, 1997-2000), HKL and SCALEPACK (Otwinowski & Minor, 1997), DENZO and SCALEPACK (Otwinowski & Minor, 1997), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX publication routines (Farrugia, 1999).

Acknowledgements

Authors are grateful to the CSIR, New Delhi, for financial assistance in the form of a JRF (AK) and a CSIR Project (NS).

References

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