metal-organic compounds
Bis[4-(dimethylamino)pyridinium] tetrabromidobis(3,4-dichlorophenyl)stannate(IV)–1-bromo-3,4-dichlorobenzene (1/1)
aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my
The Sn atom in the title substituted pyridinium stannate bromo-3,4-dichlorobenzene solvate, (C7H11N2)2[SnBr4(C6H3Cl2)2]·C6H3BrCl2, lies on a twofold axis within an octahedral C2Br4 donor set. Each cation forms an N—H⋯Br hydrogen bond to one of the Br atoms of the anion. The solvent molecule is disordered about the twofold rotation axis with equal occupancy. The crystal under investigation was non-merohedrally twinned, with a twin component ratio of 0.76:0.24.
Related literature
For bis(4-dimethylaminopyridinium) tetrahalidodiorganostannates, see: Lo & Ng (2008a,b); Yap et al. (2008). For deconvolution of the diffraction data, see: Spek (2009).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2007); cell SAINT (Bruker, 2007); data reduction: SAINT; 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: publCIF (Westrip, 2009).
Supporting information
10.1107/S1600536809017590/tk2446sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536809017590/tk2446Isup2.hkl
Tetrakis(3,4-dichlorophenyl)tin (0.70 g, 1 mol) and 4-dimethylaminopyridine hydrobromide perbromide (0.73 g, 2 mmol) were heated in ethanol/chloroform (1:1 v/v, 100 ml) for 3 h. Crystals separated from the cool solution after a day.
The presence of bromo-3,4-dichlorobenzene in the
probably arose from contamination of the tetrakis(3,4-dichlorophenyl)tin reactant, which itself was synthesized in a Grignard reaction with bromo-3,4-dichlorobenzene as the starting halogen-bearing compound.The structure initially refined to 7.7%. PLATON (Spek, 2009) gave the
as (1 0 0.746, 0 - 1 0, 0 0 - 1); a new hkl file was generated by using the detwinning tool in the program.The aromatic and pyridyl rings were refined as rigid hexagons of 1.39 Å sides. For the lattice solvent molecule, which is situated about a 2-fold axis, the C–Cl distance was restrained to 1.74±0.01 Å and the C–Br distance to 1.90±0.01 Å. The molecule was allowed to refine off the 2-fold rotation axis. The anisotropic displacement factors of the carbon atoms were restrained to be nearly isotropic.
SHELXL-97 suggested an unusually large values for a and b in the weighting scheme, and so the suggested scheme was not used. Instead, an arbitrary value of a = 0.15 was used which gave a statisfactory Goodness-of-Fit of about 1.5.
Hydrogen atoms were placed in calculated positions (C—H 0.95, N–H 0.88 Å) and were included in the
in the riding model approximation, with U(H) set to 1.2U(C,N). The torsion angles of the methyl groups were refined.The final difference Fourier map had a large peak at 1.3 Å from H7 and a deep hole at 1.5 Å from H15.
Data collection: APEX2 (Bruker, 2007); cell
SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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: publCIF (Westrip, 2009).(C7H11N2)2[SnBr4(C6H3Cl2)2]·C6H3BrCl2 | F(000) = 2312 |
Mr = 1202.55 | Dx = 2.022 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 9914 reflections |
a = 19.2308 (2) Å | θ = 2.2–28.4° |
b = 13.8983 (2) Å | µ = 6.14 mm−1 |
c = 15.4961 (2) Å | T = 100 K |
β = 107.491 (1)° | Block, colorless |
V = 3950.23 (9) Å3 | 0.25 × 0.20 × 0.15 mm |
Z = 4 |
Bruker SMART APEX diffractometer | 4495 independent reflections |
Radiation source: fine-focus sealed tube | 4061 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
ω scans | θmax = 27.5°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −24→24 |
Tmin = 0.309, Tmax = 0.459 | k = −18→18 |
17636 measured reflections | l = −20→20 |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.243 | H-atom parameters constrained |
S = 1.47 | w = 1/[σ2(Fo2) + (0.15P)2] where P = (Fo2 + 2Fc2)/3 |
4495 reflections | (Δ/σ)max = 0.001 |
225 parameters | Δρmax = 2.01 e Å−3 |
39 restraints | Δρmin = −1.80 e Å−3 |
(C7H11N2)2[SnBr4(C6H3Cl2)2]·C6H3BrCl2 | V = 3950.23 (9) Å3 |
Mr = 1202.55 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 19.2308 (2) Å | µ = 6.14 mm−1 |
b = 13.8983 (2) Å | T = 100 K |
c = 15.4961 (2) Å | 0.25 × 0.20 × 0.15 mm |
β = 107.491 (1)° |
Bruker SMART APEX diffractometer | 4495 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4061 reflections with I > 2σ(I) |
Tmin = 0.309, Tmax = 0.459 | Rint = 0.030 |
17636 measured reflections |
R[F2 > 2σ(F2)] = 0.050 | 39 restraints |
wR(F2) = 0.243 | H-atom parameters constrained |
S = 1.47 | Δρmax = 2.01 e Å−3 |
4495 reflections | Δρmin = −1.80 e Å−3 |
225 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sn1 | 0.5000 | 0.61725 (3) | 0.7500 | 0.0092 (2) | |
Br2 | 0.44267 (3) | 0.48127 (5) | 0.62311 (4) | 0.0174 (2) | |
Br1 | 0.44630 (3) | 0.75638 (5) | 0.62507 (4) | 0.0186 (2) | |
Cl1 | 0.81264 (8) | 0.62573 (10) | 0.85386 (12) | 0.0179 (4) | |
Cl2 | 0.81408 (10) | 0.62116 (11) | 0.65044 (13) | 0.0243 (4) | |
N2 | 0.2115 (3) | 0.6236 (4) | 0.1836 (4) | 0.0196 (12) | |
C1 | 0.60066 (16) | 0.6174 (2) | 0.7153 (3) | 0.0102 (11) | |
C2 | 0.6660 (2) | 0.6216 (2) | 0.7850 (2) | 0.0102 (11) | |
H2 | 0.6657 | 0.6238 | 0.8461 | 0.012* | |
C3 | 0.73187 (16) | 0.6224 (2) | 0.7651 (2) | 0.0138 (12) | |
C4 | 0.73233 (17) | 0.6191 (3) | 0.6756 (3) | 0.0155 (13) | |
C5 | 0.6670 (2) | 0.6150 (3) | 0.6060 (2) | 0.0151 (13) | |
H5 | 0.6673 | 0.6128 | 0.5449 | 0.018* | |
C6 | 0.60113 (17) | 0.6142 (2) | 0.6259 (2) | 0.0175 (13) | |
H6 | 0.5564 | 0.6113 | 0.5783 | 0.021* | |
N1 | 0.3539 (2) | 0.6345 (3) | 0.4428 (2) | 0.0293 (14) | |
H1 | 0.3842 | 0.6371 | 0.4981 | 0.035* | |
C7 | 0.38080 (17) | 0.6245 (3) | 0.3695 (3) | 0.0244 (16) | |
H7 | 0.4319 | 0.6205 | 0.3790 | 0.029* | |
C8 | 0.3330 (2) | 0.6204 (3) | 0.2822 (3) | 0.0185 (14) | |
H8 | 0.3514 | 0.6135 | 0.2320 | 0.022* | |
C9 | 0.2582 (2) | 0.6262 (3) | 0.2682 (2) | 0.0144 (12) | |
C10 | 0.23132 (17) | 0.6362 (3) | 0.3415 (3) | 0.0185 (13) | |
H10 | 0.1802 | 0.6401 | 0.3320 | 0.022* | |
C11 | 0.2791 (2) | 0.6403 (3) | 0.4288 (2) | 0.0239 (14) | |
H11 | 0.2608 | 0.6471 | 0.4790 | 0.029* | |
C12 | 0.2386 (5) | 0.6177 (5) | 0.1057 (5) | 0.0273 (17) | |
H12A | 0.2695 | 0.6737 | 0.1050 | 0.041* | |
H12B | 0.1974 | 0.6168 | 0.0501 | 0.041* | |
H12C | 0.2672 | 0.5587 | 0.1095 | 0.041* | |
C13 | 0.1323 (4) | 0.6238 (5) | 0.1685 (6) | 0.0268 (17) | |
H13A | 0.1196 | 0.5727 | 0.2047 | 0.040* | |
H13B | 0.1071 | 0.6126 | 0.1043 | 0.040* | |
H13C | 0.1175 | 0.6862 | 0.1866 | 0.040* | |
Br3 | 0.5258 (5) | 0.7963 (5) | 0.4343 (4) | 0.0355 (11) | 0.50 |
Cl3 | 0.4624 (2) | 0.9970 (3) | 0.0505 (2) | 0.0351 (9) | 0.50 |
Cl4 | 0.4620 (14) | 0.7751 (14) | 0.0633 (11) | 0.038 (3) | 0.50 |
C14 | 0.5139 (16) | 0.8551 (8) | 0.3234 (8) | 0.027 (4) | 0.50 |
C15 | 0.501 (2) | 0.7983 (4) | 0.2464 (11) | 0.027 (3) | 0.50 |
H15 | 0.5033 | 0.7302 | 0.2517 | 0.032* | 0.50 |
C16 | 0.4852 (16) | 0.8411 (7) | 0.1616 (9) | 0.025 (4) | 0.50 |
C17 | 0.4820 (8) | 0.9408 (8) | 0.1538 (4) | 0.023 (4) | 0.50 |
C18 | 0.4948 (9) | 0.9976 (4) | 0.2309 (6) | 0.023 (4) | 0.50 |
H18 | 0.4926 | 1.0657 | 0.2255 | 0.028* | 0.50 |
C19 | 0.5107 (8) | 0.9548 (8) | 0.3156 (4) | 0.021 (3) | 0.50 |
H19 | 0.5194 | 0.9936 | 0.3683 | 0.025* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.0068 (4) | 0.0113 (4) | 0.0099 (3) | 0.000 | 0.0031 (2) | 0.000 |
Br2 | 0.0141 (4) | 0.0186 (4) | 0.0195 (4) | −0.0016 (2) | 0.0048 (3) | −0.0054 (2) |
Br1 | 0.0175 (4) | 0.0215 (4) | 0.0169 (4) | 0.0013 (2) | 0.0050 (3) | 0.0030 (2) |
Cl1 | 0.0082 (7) | 0.0195 (8) | 0.0236 (8) | 0.0003 (5) | 0.0010 (6) | −0.0001 (5) |
Cl2 | 0.0133 (8) | 0.0351 (10) | 0.0291 (9) | −0.0020 (5) | 0.0132 (7) | −0.0020 (6) |
N2 | 0.019 (3) | 0.019 (3) | 0.018 (3) | 0.0001 (18) | 0.001 (2) | 0.0001 (19) |
C1 | 0.011 (3) | 0.009 (3) | 0.011 (3) | 0.0016 (17) | 0.003 (2) | 0.0001 (17) |
C2 | 0.007 (3) | 0.014 (3) | 0.010 (3) | 0.0001 (17) | 0.003 (2) | −0.0007 (18) |
C3 | 0.008 (3) | 0.014 (3) | 0.019 (3) | −0.0021 (18) | 0.004 (2) | −0.001 (2) |
C4 | 0.008 (3) | 0.015 (3) | 0.026 (4) | −0.0011 (18) | 0.008 (3) | 0.000 (2) |
C5 | 0.016 (3) | 0.017 (3) | 0.014 (3) | −0.003 (2) | 0.007 (2) | −0.002 (2) |
C6 | 0.018 (3) | 0.019 (3) | 0.016 (3) | −0.002 (2) | 0.006 (3) | −0.002 (2) |
N1 | 0.027 (4) | 0.033 (3) | 0.018 (3) | 0.008 (2) | −0.007 (3) | −0.007 (2) |
C7 | 0.016 (3) | 0.018 (3) | 0.033 (4) | 0.003 (2) | −0.002 (3) | −0.006 (3) |
C8 | 0.016 (3) | 0.016 (3) | 0.023 (3) | 0.001 (2) | 0.007 (3) | −0.002 (2) |
C9 | 0.017 (3) | 0.012 (3) | 0.014 (3) | −0.002 (2) | 0.003 (2) | −0.0018 (19) |
C10 | 0.015 (3) | 0.013 (3) | 0.027 (3) | 0.000 (2) | 0.006 (3) | 0.001 (2) |
C11 | 0.033 (4) | 0.026 (3) | 0.012 (3) | 0.008 (3) | 0.007 (3) | −0.002 (3) |
C12 | 0.036 (5) | 0.031 (4) | 0.011 (3) | 0.001 (3) | 0.001 (3) | 0.001 (2) |
C13 | 0.013 (4) | 0.032 (4) | 0.030 (4) | 0.001 (2) | −0.002 (3) | −0.004 (3) |
Br3 | 0.050 (3) | 0.036 (3) | 0.0186 (11) | −0.0140 (19) | 0.0077 (13) | −0.0007 (11) |
Cl3 | 0.049 (2) | 0.0289 (19) | 0.0208 (16) | −0.0123 (16) | −0.0002 (15) | 0.0031 (14) |
Cl4 | 0.047 (7) | 0.039 (8) | 0.026 (3) | 0.008 (4) | 0.009 (3) | −0.003 (3) |
C14 | 0.030 (8) | 0.036 (7) | 0.017 (6) | −0.012 (7) | 0.012 (6) | 0.003 (6) |
C15 | 0.028 (5) | 0.024 (5) | 0.032 (5) | 0.003 (9) | 0.014 (4) | −0.008 (9) |
C16 | 0.018 (7) | 0.039 (8) | 0.027 (6) | 0.014 (6) | 0.018 (6) | 0.001 (6) |
C17 | 0.024 (6) | 0.028 (7) | 0.020 (7) | −0.007 (5) | 0.012 (5) | −0.009 (6) |
C18 | 0.026 (6) | 0.025 (5) | 0.019 (9) | 0.003 (5) | 0.007 (7) | 0.000 (4) |
C19 | 0.022 (6) | 0.022 (6) | 0.023 (7) | −0.007 (5) | 0.015 (6) | 0.000 (6) |
Sn1—C1i | 2.159 (3) | C8—C9 | 1.3900 |
Sn1—C1 | 2.159 (3) | C8—H8 | 0.9500 |
Sn1—Br2 | 2.7111 (7) | C9—C10 | 1.3900 |
Sn1—Br2i | 2.7111 (7) | C10—C11 | 1.3900 |
Sn1—Br1i | 2.7114 (7) | C10—H10 | 0.9500 |
Sn1—Br1 | 2.7114 (7) | C11—H11 | 0.9500 |
Cl1—C3 | 1.739 (3) | C12—H12A | 0.9800 |
Cl2—C4 | 1.730 (3) | C12—H12B | 0.9800 |
N2—C9 | 1.349 (7) | C12—H12C | 0.9800 |
N2—C12 | 1.454 (10) | C13—H13A | 0.9800 |
N2—C13 | 1.468 (10) | C13—H13B | 0.9800 |
C1—C2 | 1.3900 | C13—H13C | 0.9800 |
C1—C6 | 1.3900 | Br3—C14 | 1.855 (6) |
C2—C3 | 1.3900 | Cl3—C17 | 1.719 (7) |
C2—H2 | 0.9500 | Cl4—C16 | 1.718 (9) |
C3—C4 | 1.3900 | C14—C15 | 1.3900 |
C4—C5 | 1.3900 | C14—C19 | 1.3900 |
C5—C6 | 1.3900 | C15—C16 | 1.3900 |
C5—H5 | 0.9500 | C15—H15 | 0.9500 |
C6—H6 | 0.9500 | C16—C17 | 1.3900 |
N1—C7 | 1.3900 | C17—C18 | 1.3900 |
N1—C11 | 1.3900 | C18—C19 | 1.3900 |
N1—H1 | 0.8800 | C18—H18 | 0.9500 |
C7—C8 | 1.3900 | C19—H19 | 0.9500 |
C7—H7 | 0.9500 | ||
C1i—Sn1—C1 | 179.87 (18) | C7—C8—C9 | 120.0 |
C1i—Sn1—Br2 | 88.95 (10) | C7—C8—H8 | 120.0 |
C1—Sn1—Br2 | 91.15 (10) | C9—C8—H8 | 120.0 |
C1i—Sn1—Br2i | 91.15 (10) | N2—C9—C8 | 120.4 (4) |
C1—Sn1—Br2i | 88.95 (10) | N2—C9—C10 | 119.6 (4) |
Br2—Sn1—Br2i | 91.62 (3) | C8—C9—C10 | 120.0 |
C1i—Sn1—Br1i | 89.95 (10) | C11—C10—C9 | 120.0 |
C1—Sn1—Br1i | 89.95 (10) | C11—C10—H10 | 120.0 |
Br2—Sn1—Br1i | 178.301 (19) | C9—C10—H10 | 120.0 |
Br2i—Sn1—Br1i | 89.70 (2) | C10—C11—N1 | 120.0 |
C1i—Sn1—Br1 | 89.95 (10) | C10—C11—H11 | 120.0 |
C1—Sn1—Br1 | 89.95 (10) | N1—C11—H11 | 120.0 |
Br2—Sn1—Br1 | 89.70 (2) | N2—C12—H12A | 109.5 |
Br2i—Sn1—Br1 | 178.301 (19) | N2—C12—H12B | 109.5 |
Br1i—Sn1—Br1 | 89.01 (3) | H12A—C12—H12B | 109.5 |
C9—N2—C12 | 120.5 (6) | N2—C12—H12C | 109.5 |
C9—N2—C13 | 120.7 (6) | H12A—C12—H12C | 109.5 |
C12—N2—C13 | 118.8 (6) | H12B—C12—H12C | 109.5 |
C2—C1—C6 | 120.0 | N2—C13—H13A | 109.5 |
C2—C1—Sn1 | 118.5 (2) | N2—C13—H13B | 109.5 |
C6—C1—Sn1 | 121.5 (2) | H13A—C13—H13B | 109.5 |
C3—C2—C1 | 120.0 | N2—C13—H13C | 109.5 |
C3—C2—H2 | 120.0 | H13A—C13—H13C | 109.5 |
C1—C2—H2 | 120.0 | H13B—C13—H13C | 109.5 |
C2—C3—C4 | 120.0 | C15—C14—C19 | 120.0 |
C2—C3—Cl1 | 118.8 (2) | C15—C14—Br3 | 119.1 (9) |
C4—C3—Cl1 | 121.2 (2) | C19—C14—Br3 | 120.6 (9) |
C5—C4—C3 | 120.0 | C16—C15—C14 | 120.0 |
C5—C4—Cl2 | 119.8 (2) | C16—C15—H15 | 120.0 |
C3—C4—Cl2 | 120.2 (2) | C14—C15—H15 | 120.0 |
C4—C5—C6 | 120.0 | C15—C16—C17 | 120.0 |
C4—C5—H5 | 120.0 | C15—C16—Cl4 | 122.3 (11) |
C6—C5—H5 | 120.0 | C17—C16—Cl4 | 117.6 (11) |
C5—C6—C1 | 120.0 | C18—C17—C16 | 120.0 |
C5—C6—H6 | 120.0 | C18—C17—Cl3 | 118.3 (8) |
C1—C6—H6 | 120.0 | C16—C17—Cl3 | 121.7 (8) |
C7—N1—C11 | 120.0 | C17—C18—C19 | 120.0 |
C7—N1—H1 | 120.0 | C17—C18—H18 | 120.0 |
C11—N1—H1 | 120.0 | C19—C18—H18 | 120.0 |
C8—C7—N1 | 120.0 | C18—C19—C14 | 120.0 |
C8—C7—H7 | 120.0 | C18—C19—H19 | 120.0 |
N1—C7—H7 | 120.0 | C14—C19—H19 | 120.0 |
Br2—Sn1—C1—C2 | −138.45 (15) | C12—N2—C9—C8 | −1.9 (6) |
Br2i—Sn1—C1—C2 | −46.86 (16) | C13—N2—C9—C8 | 176.2 (4) |
Br1i—Sn1—C1—C2 | 42.84 (16) | C12—N2—C9—C10 | 177.2 (4) |
Br1—Sn1—C1—C2 | 131.85 (16) | C13—N2—C9—C10 | −4.7 (6) |
Br2—Sn1—C1—C6 | 41.96 (17) | C7—C8—C9—N2 | 179.0 (4) |
Br2i—Sn1—C1—C6 | 133.56 (17) | C7—C8—C9—C10 | 0.0 |
Br1i—Sn1—C1—C6 | −136.74 (17) | N2—C9—C10—C11 | −179.0 (4) |
Br1—Sn1—C1—C6 | −47.73 (17) | C8—C9—C10—C11 | 0.0 |
C6—C1—C2—C3 | 0.0 | C9—C10—C11—N1 | 0.0 |
Sn1—C1—C2—C3 | −179.6 (2) | C7—N1—C11—C10 | 0.0 |
C1—C2—C3—C4 | 0.0 | C19—C14—C15—C16 | 0.0 |
C1—C2—C3—Cl1 | −179.0 (2) | Br3—C14—C15—C16 | 173.9 (18) |
C2—C3—C4—C5 | 0.0 | C14—C15—C16—C17 | 0.0 |
Cl1—C3—C4—C5 | 179.0 (3) | C14—C15—C16—Cl4 | −175 (2) |
C2—C3—C4—Cl2 | 179.5 (3) | C15—C16—C17—C18 | 0.0 |
Cl1—C3—C4—Cl2 | −1.5 (3) | Cl4—C16—C17—C18 | 175.1 (19) |
C3—C4—C5—C6 | 0.0 | C15—C16—C17—Cl3 | −179.9 (11) |
Cl2—C4—C5—C6 | −179.5 (3) | Cl4—C16—C17—Cl3 | −5 (2) |
C4—C5—C6—C1 | 0.0 | C16—C17—C18—C19 | 0.0 |
C2—C1—C6—C5 | 0.0 | Cl3—C17—C18—C19 | 179.9 (10) |
Sn1—C1—C6—C5 | 179.6 (2) | C17—C18—C19—C14 | 0.0 |
C11—N1—C7—C8 | 0.0 | C15—C14—C19—C18 | 0.0 |
N1—C7—C8—C9 | 0.0 | Br3—C14—C19—C18 | −173.8 (18) |
Symmetry code: (i) −x+1, y, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | (C7H11N2)2[SnBr4(C6H3Cl2)2]·C6H3BrCl2 |
Mr | 1202.55 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 100 |
a, b, c (Å) | 19.2308 (2), 13.8983 (2), 15.4961 (2) |
β (°) | 107.491 (1) |
V (Å3) | 3950.23 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 6.14 |
Crystal size (mm) | 0.25 × 0.20 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART APEX diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.309, 0.459 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 17636, 4495, 4061 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.243, 1.47 |
No. of reflections | 4495 |
No. of parameters | 225 |
No. of restraints | 39 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.01, −1.80 |
Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2009).
Acknowledgements
We thank the University of Malaya for funding this study (RG020/09AFR).
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