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Tripotassium bis­­(acetato-κ2O,O′)(thio­cyanato-κN)plumbate(II) di­thio­cyanate

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

(Received 2 June 2009; accepted 5 June 2009; online 10 June 2009)

In the crystal structure of the title salt, K3[Pb(CH3COO)2(NCS)](NCS)2, the [Pb(CH3COO)2(NCS)] anion exists as a covalently bonded entity in which the acetate anions chelate in an anisobidentate manner. The Pb atom shows a distorted ψ-octa­hedral coordination to four acetate O atoms and one isocyanate N atom, with the stereochemically active lone pair occupying one of the six sites. When the three longer Pb⋯S inter­actions are considered, the eight-coordinate geometry is based on a dodeca­hedron. The Pb(CH3COO)2(NCS)] anion has mirror symmetry. The potassium cations connect the other constituents into a three-dimensional network through electrostatic K⋯N and K⋯S inter­actions.

Related literature

In [K6Pb6(CH3CO2)12(NCS)2](NCS)4, the acetate groups link the lead(II) atoms into a chain; see: Morsali & Mahjoub (2004[Morsali, A. & Mahjoub, A. R. (2004). Helv. Chim. Acta, 87, 2717-2722.]).

[Scheme 1]

Experimental

Crystal data
  • K3[Pb(C2H3O2)2(NCS)](NCS)2

  • Mr = 616.82

  • Monoclinic, P 21 /m

  • a = 6.1968 (1) Å

  • b = 19.2499 (3) Å

  • c = 7.6354 (1) Å

  • β = 106.982 (1)°

  • V = 871.10 (2) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 10.77 mm−1

  • T = 140 K

  • 0.25 × 0.20 × 0.08 mm

Data collection
  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.174, Tmax = 0.480 (expected range = 0.153–0.422)

  • 6058 measured reflections

  • 2045 independent reflections

  • 2015 reflections with I > 2σ(I)

  • Rint = 0.023

Refinement
  • R[F2 > 2σ(F2)] = 0.022

  • wR(F2) = 0.056

  • S = 1.16

  • 2045 reflections

  • 104 parameters

  • H-atom parameters constrained

  • Δρmax = 0.81 e Å−3

  • Δρmin = −2.00 e Å−3

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2009[Westrip, S. P. (2009). publCIF. In preparation.]).

Supporting information


Related literature top

In [K6Pb6(CH3CO2)12(NCS)2](NCS)4, the acetate groups link the lead(II) atoms into a chain; see: Morsali & Mahjoub (2004).

Experimental top

2,4-Diamino-6-(1-piperidinyl)-2,4-pyrimidine N-oxide (commercial name: minoxidil) (0.5 mmol, 0.10 g), lead(II) acetate (0.5 mmol, 0.17 g) and potassium thiocyanate (1 mmol, 0.10 g) were dissolved in methanol (100 ml). The solution was concentrated to a smaller volume and this was mixed with a similar volume of chloroform. Colorless prisms separated after several days.

Refinement top

Hydrogen atoms were placed at calculated positions (C–H 0.98 Å) and were treated as riding on the carbon atom with U(H) set to 1.5Ueq(C). The final difference Fourier map had a deep hole at 1 Å from N1.

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (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: publCIF (Westrip, 2009).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of a portion of the polymeric structure of K3Pb(NCS)3(CH3CO2)2 at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. Symmetry operation i: x, 1.5-y, z.
[Figure 2] Fig. 2. Detail showing the dodecahedral geometry of the Pb(II) atom.
Tripotassium bis(acetato-κ2O,O')(thiocyanato-κN)plumbate(II) dithiocyanate top
Crystal data top
K3[Pb(C2H3O2)2(NCS)](NCS)2F(000) = 576
Mr = 616.82Dx = 2.352 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 4971 reflections
a = 6.1968 (1) Åθ = 2.9–28.3°
b = 19.2499 (3) ŵ = 10.77 mm1
c = 7.6354 (1) ÅT = 140 K
β = 106.982 (1)°Block, colorless
V = 871.10 (2) Å30.25 × 0.20 × 0.08 mm
Z = 2
Data collection top
Bruker SMART APEX
diffractometer
2045 independent reflections
Radiation source: fine-focus sealed tube2015 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 78
Tmin = 0.174, Tmax = 0.480k = 2525
6058 measured reflectionsl = 99
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056H-atom parameters constrained
S = 1.16 w = 1/[σ2(Fo2) + (0.03P)2 + 1.3438P]
where P = (Fo2 + 2Fc2)/3
2045 reflections(Δ/σ)max = 0.001
104 parametersΔρmax = 0.81 e Å3
0 restraintsΔρmin = 2.00 e Å3
Crystal data top
K3[Pb(C2H3O2)2(NCS)](NCS)2V = 871.10 (2) Å3
Mr = 616.82Z = 2
Monoclinic, P21/mMo Kα radiation
a = 6.1968 (1) ŵ = 10.77 mm1
b = 19.2499 (3) ÅT = 140 K
c = 7.6354 (1) Å0.25 × 0.20 × 0.08 mm
β = 106.982 (1)°
Data collection top
Bruker SMART APEX
diffractometer
2045 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
2015 reflections with I > 2σ(I)
Tmin = 0.174, Tmax = 0.480Rint = 0.023
6058 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0220 restraints
wR(F2) = 0.056H-atom parameters constrained
S = 1.16Δρmax = 0.81 e Å3
2045 reflectionsΔρmin = 2.00 e Å3
104 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.41686 (3)0.75000.47400 (2)0.01158 (7)
K10.85392 (14)0.59423 (4)0.42518 (12)0.01948 (17)
K20.74409 (19)0.75000.09371 (15)0.0160 (2)
S11.1475 (2)0.75000.8492 (2)0.0247 (3)
S20.65682 (16)0.62677 (5)0.76528 (14)0.01949 (19)
N10.8449 (7)0.75000.4972 (6)0.0151 (9)
N20.2738 (6)0.54336 (19)0.6214 (6)0.0289 (8)
O10.4696 (4)0.66654 (13)0.2532 (4)0.0162 (5)
O20.1161 (4)0.66405 (13)0.2588 (4)0.0171 (5)
C10.2743 (6)0.63941 (18)0.2063 (5)0.0146 (7)
C20.2360 (7)0.5741 (2)0.0917 (6)0.0236 (8)
H2A0.22830.53410.16890.035*
H2B0.36090.56780.03880.035*
H2C0.09400.57820.00690.035*
C30.9724 (8)0.75000.6432 (7)0.0142 (10)
C40.4309 (6)0.57822 (19)0.6821 (5)0.0180 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.01294 (11)0.01291 (10)0.01004 (11)0.0000.00516 (7)0.000
K10.0164 (4)0.0153 (4)0.0286 (4)0.0018 (3)0.0095 (3)0.0037 (3)
K20.0168 (5)0.0192 (5)0.0129 (5)0.0000.0058 (4)0.000
S10.0184 (6)0.0388 (8)0.0144 (6)0.0000.0011 (5)0.000
S20.0194 (4)0.0185 (4)0.0210 (5)0.0041 (3)0.0065 (4)0.0016 (4)
N10.0119 (19)0.020 (2)0.013 (2)0.0000.0035 (17)0.000
N20.0217 (18)0.0232 (17)0.036 (2)0.0019 (14)0.0000 (16)0.0014 (15)
O10.0136 (12)0.0192 (12)0.0162 (13)0.0004 (9)0.0050 (10)0.0031 (10)
O20.0142 (12)0.0194 (12)0.0191 (13)0.0017 (9)0.0071 (10)0.0002 (10)
C10.0171 (16)0.0143 (15)0.0107 (16)0.0017 (12)0.0015 (13)0.0049 (13)
C20.0234 (19)0.0199 (18)0.025 (2)0.0010 (15)0.0034 (17)0.0079 (16)
C30.012 (2)0.012 (2)0.020 (3)0.0000.008 (2)0.000
C40.0175 (18)0.0142 (16)0.0205 (19)0.0032 (13)0.0031 (15)0.0034 (14)
Geometric parameters (Å, º) top
Pb1—O12.419 (3)K2—S2vi3.3788 (13)
Pb1—O1i2.419 (3)K2—S2vii3.3788 (13)
Pb1—O22.669 (3)S1—C31.630 (5)
Pb1—O2i2.669 (3)S2—C41.649 (4)
Pb1—N12.606 (4)S2—K2viii3.3788 (13)
Pb1—S1ii3.713 (1)N1—C31.163 (7)
Pb1—S23.294 (1)N1—K1i3.0520 (12)
Pb1—S2i3.294 (1)N2—C41.162 (5)
K1—O2iii2.696 (3)N2—K1iv2.757 (4)
K1—O12.740 (3)N2—K1ii2.774 (4)
K1—N2iv2.757 (4)O1—C11.270 (4)
K1—N2iii2.774 (4)O2—C11.255 (5)
K1—N13.0520 (12)O2—K1ii2.696 (3)
K1—S23.2373 (13)O2—K2ii2.818 (3)
K2—O2v2.818 (3)C1—C21.509 (5)
K2—O2iii2.818 (3)C2—H2A0.9800
K2—O12.858 (3)C2—H2B0.9800
K2—O1i2.858 (3)C2—H2C0.9800
K2—N12.959 (5)C3—K1i3.404 (3)
O1—Pb1—O1i83.23 (13)O2v—K2—S1ix143.98 (5)
O1—Pb1—N172.87 (9)O2iii—K2—S1ix143.98 (5)
O1i—Pb1—N172.87 (9)O1—K2—S1ix64.83 (6)
O1—Pb1—O251.04 (8)O1i—K2—S1ix64.83 (6)
O1i—Pb1—O2101.23 (8)N1—K2—S1ix114.20 (9)
N1—Pb1—O2123.76 (9)S2vi—K2—S1ix72.51 (3)
O1—Pb1—O2i101.23 (8)S2vii—K2—S1ix72.51 (3)
O1i—Pb1—O2i51.04 (8)S1vi—K2—S1ix120.08 (5)
N1—Pb1—O2i123.76 (9)C3—S1—K2viii97.79 (19)
O2—Pb1—O2i76.62 (11)C3—S1—K2x142.1 (2)
O2iii—K1—O194.59 (8)K2viii—S1—K2x120.08 (5)
O2iii—K1—N2iv127.44 (11)C4—S2—K193.34 (15)
O1—K1—N2iv104.45 (9)C4—S2—K2viii128.15 (15)
O2iii—K1—N2iii80.28 (10)K1—S2—K2viii135.65 (4)
O1—K1—N2iii170.07 (10)C3—N1—Pb1117.3 (4)
N2iv—K1—N2iii85.36 (11)C3—N1—K2151.1 (4)
O2iii—K1—N168.92 (10)Pb1—N1—K291.61 (13)
O1—K1—N161.85 (10)C3—N1—K197.45 (9)
N2iv—K1—N1161.31 (12)Pb1—N1—K193.42 (8)
N2iii—K1—N1108.25 (11)K2—N1—K179.74 (8)
O2iii—K1—S2134.60 (6)C3—N1—K1i97.45 (9)
O1—K1—S278.90 (6)Pb1—N1—K1i93.42 (8)
N2iv—K1—S297.35 (9)K2—N1—K1i79.74 (8)
N2iii—K1—S298.58 (9)K1—N1—K1i158.52 (17)
N1—K1—S268.55 (9)C4—N2—K1iv141.4 (3)
O2v—K2—O2iii71.90 (11)C4—N2—K1ii123.8 (3)
O2v—K2—O1130.58 (9)K1iv—N2—K1ii94.64 (11)
O2iii—K2—O189.45 (8)C1—O1—Pb199.1 (2)
O2v—K2—O1i89.45 (8)C1—O1—K1123.3 (2)
O2iii—K2—O1i130.58 (9)Pb1—O1—K1106.18 (9)
O1—K2—O1i68.41 (10)C1—O1—K2138.4 (2)
O2v—K2—N168.78 (9)Pb1—O1—K298.16 (8)
O2iii—K2—N168.78 (9)K1—O1—K286.99 (8)
O1—K2—N161.80 (9)C1—O2—Pb187.8 (2)
O1i—K2—N161.80 (9)C1—O2—K1ii126.6 (2)
O2v—K2—S2vi132.59 (7)Pb1—O2—K1ii115.30 (10)
O2iii—K2—S2vi81.51 (6)C1—O2—K2ii133.8 (2)
O1—K2—S2vi86.29 (6)Pb1—O2—K2ii104.14 (8)
O1i—K2—S2vi136.45 (7)K1ii—O2—K2ii88.66 (8)
N1—K2—S2vi135.40 (2)O2—C1—O1121.6 (3)
O2v—K2—S2vii81.51 (6)O2—C1—C2119.6 (3)
O2iii—K2—S2vii132.59 (7)O1—C1—C2118.8 (3)
O1—K2—S2vii136.45 (6)C1—C2—H2A109.5
O1i—K2—S2vii86.29 (6)C1—C2—H2B109.5
N1—K2—S2vii135.40 (2)H2A—C2—H2B109.5
S2vi—K2—S2vii89.19 (4)C1—C2—H2C109.5
O2v—K2—S1vi67.87 (6)H2A—C2—H2C109.5
O2iii—K2—S1vi67.87 (6)H2B—C2—H2C109.5
O1—K2—S1vi145.78 (5)N1—C3—S1179.1 (5)
O1i—K2—S1vi145.78 (5)N1—C3—K1i62.76 (9)
N1—K2—S1vi125.72 (9)S1—C3—K1i117.37 (8)
S2vi—K2—S1vi65.92 (3)N2—C4—S2178.7 (4)
S2vii—K2—S1vi65.92 (3)
O2iii—K1—S2—C4150.92 (15)O1i—Pb1—O1—C1114.5 (2)
O1—K1—S2—C465.45 (14)N1—Pb1—O1—C1171.4 (2)
N2iv—K1—S2—C437.91 (15)O2—Pb1—O1—C14.14 (19)
N2iii—K1—S2—C4124.30 (15)O2i—Pb1—O1—C166.5 (2)
N1—K1—S2—C4129.38 (15)O1i—Pb1—O1—K1116.73 (7)
O2iii—K1—S2—K2viii9.98 (11)N1—Pb1—O1—K142.61 (10)
O1—K1—S2—K2viii95.45 (7)O2—Pb1—O1—K1132.90 (14)
N2iv—K1—S2—K2viii161.19 (9)O2i—Pb1—O1—K1164.73 (9)
N2iii—K1—S2—K2viii74.80 (9)O1i—Pb1—O1—K227.51 (11)
N1—K1—S2—K2viii31.52 (10)N1—Pb1—O1—K246.61 (9)
O1—Pb1—N1—C3135.98 (7)O2—Pb1—O1—K2137.88 (13)
O1i—Pb1—N1—C3135.98 (7)O2i—Pb1—O1—K275.51 (9)
O2—Pb1—N1—C3131.78 (8)O2iii—K1—O1—C1145.2 (3)
O2i—Pb1—N1—C3131.78 (8)N2iv—K1—O1—C114.7 (3)
O1—Pb1—N1—K244.02 (7)N1—K1—O1—C1151.6 (3)
O1i—Pb1—N1—K244.02 (7)S2—K1—O1—C180.2 (3)
O2—Pb1—N1—K248.22 (8)O2iii—K1—O1—Pb1101.92 (10)
O2i—Pb1—N1—K248.22 (8)N2iv—K1—O1—Pb1127.50 (12)
O1—Pb1—N1—K135.79 (10)N1—K1—O1—Pb138.80 (11)
O1i—Pb1—N1—K1123.83 (13)S2—K1—O1—Pb132.68 (7)
O2—Pb1—N1—K131.60 (15)O2iii—K1—O1—K24.30 (8)
O2i—Pb1—N1—K1128.03 (8)N2iv—K1—O1—K2134.88 (10)
O1—Pb1—N1—K1i123.83 (13)N1—K1—O1—K258.82 (11)
O1i—Pb1—N1—K1i35.79 (10)S2—K1—O1—K2130.30 (6)
O2—Pb1—N1—K1i128.03 (8)O2v—K2—O1—C1158.4 (3)
O2i—Pb1—N1—K1i31.60 (15)O2iii—K2—O1—C1136.3 (3)
O2v—K2—N1—C339.03 (6)O1i—K2—O1—C189.0 (3)
O2iii—K2—N1—C339.03 (6)N1—K2—O1—C1157.7 (4)
O1—K2—N1—C3140.36 (6)S2vi—K2—O1—C154.7 (3)
O1i—K2—N1—C3140.36 (7)S2vii—K2—O1—C130.2 (4)
S2vi—K2—N1—C390.78 (10)S1vi—K2—O1—C189.4 (4)
S2vii—K2—N1—C390.78 (10)S1ix—K2—O1—C117.7 (3)
S1vi—K2—N1—C30.000 (2)O2v—K2—O1—Pb144.69 (13)
S1ix—K2—N1—C3180.000 (3)O2iii—K2—O1—Pb1110.02 (9)
O2v—K2—N1—Pb1140.97 (6)O1i—K2—O1—Pb124.68 (10)
O2iii—K2—N1—Pb1140.97 (6)N1—K2—O1—Pb143.94 (8)
O1—K2—N1—Pb139.64 (6)S2vi—K2—O1—Pb1168.45 (8)
O1i—K2—N1—Pb139.64 (6)S2vii—K2—O1—Pb183.54 (10)
S2vi—K2—N1—Pb189.22 (10)S1vi—K2—O1—Pb1156.87 (8)
S2vii—K2—N1—Pb189.22 (10)S1ix—K2—O1—Pb196.05 (8)
S1vi—K2—N1—Pb1180.0O2v—K2—O1—K161.24 (11)
S1ix—K2—N1—Pb10.0O2iii—K2—O1—K14.10 (8)
O2v—K2—N1—K1125.85 (11)O1i—K2—O1—K1130.60 (4)
O2iii—K2—N1—K147.79 (8)N1—K2—O1—K161.98 (8)
O1—K2—N1—K153.55 (7)S2vi—K2—O1—K185.63 (6)
O1i—K2—N1—K1132.82 (11)S2vii—K2—O1—K1170.54 (5)
S2vi—K2—N1—K13.96 (16)S1vi—K2—O1—K150.94 (14)
S2vii—K2—N1—K1177.60 (6)S1ix—K2—O1—K1158.03 (8)
S1vi—K2—N1—K186.82 (7)O1—Pb1—O2—C14.13 (19)
S1ix—K2—N1—K193.18 (7)O1i—Pb1—O2—C175.8 (2)
O2v—K2—N1—K1i47.79 (8)N1—Pb1—O2—C11.0 (2)
O2iii—K2—N1—K1i125.85 (11)O2i—Pb1—O2—C1120.85 (18)
O1—K2—N1—K1i132.82 (11)O1—Pb1—O2—K1ii134.06 (15)
O1i—K2—N1—K1i53.55 (7)O1i—Pb1—O2—K1ii154.31 (10)
S2vi—K2—N1—K1i177.60 (6)N1—Pb1—O2—K1ii128.90 (11)
S2vii—K2—N1—K1i3.96 (16)O2i—Pb1—O2—K1ii109.23 (8)
S1vi—K2—N1—K1i86.82 (7)O1—Pb1—O2—K2ii130.64 (13)
S1ix—K2—N1—K1i93.18 (7)O1i—Pb1—O2—K2ii59.01 (10)
O2iii—K1—N1—C3100.2 (4)N1—Pb1—O2—K2ii135.80 (10)
O1—K1—N1—C3152.1 (4)O2i—Pb1—O2—K2ii13.92 (12)
N2iv—K1—N1—C3106.4 (5)Pb1—O2—C1—O17.2 (3)
N2iii—K1—N1—C328.7 (4)K1ii—O2—C1—O1127.5 (3)
S2—K1—N1—C363.5 (3)K2ii—O2—C1—O1100.3 (4)
O2iii—K1—N1—Pb1141.70 (14)Pb1—O2—C1—C2170.0 (3)
O1—K1—N1—Pb134.03 (9)K1ii—O2—C1—C249.7 (4)
N2iv—K1—N1—Pb111.7 (4)K2ii—O2—C1—C282.5 (4)
N2iii—K1—N1—Pb1146.82 (12)Pb1—O1—C1—O28.0 (4)
S2—K1—N1—Pb154.57 (9)K1—O1—C1—O2124.4 (3)
O2iii—K1—N1—K250.68 (9)K2—O1—C1—O2105.3 (4)
O1—K1—N1—K256.99 (9)Pb1—O1—C1—C2169.2 (3)
N2iv—K1—N1—K2102.7 (4)K1—O1—C1—C252.9 (4)
N2iii—K1—N1—K2122.16 (11)K2—O1—C1—C277.4 (4)
S2—K1—N1—K2145.59 (10)Pb1—N1—C3—K1i97.76 (12)
O2iii—K1—N1—K1i33.4 (4)K2—N1—C3—K1i82.24 (12)
O1—K1—N1—K1i74.3 (4)K1—N1—C3—K1i164.5 (2)
N2iv—K1—N1—K1i120.0 (5)K2viii—S1—C3—K1i97.27 (19)
N2iii—K1—N1—K1i104.8 (4)K2x—S1—C3—K1i82.73 (19)
S2—K1—N1—K1i162.9 (5)
Symmetry codes: (i) x, y+3/2, z; (ii) x1, y, z; (iii) x+1, y, z; (iv) x+1, y+1, z+1; (v) x+1, y+3/2, z; (vi) x, y, z1; (vii) x, y+3/2, z1; (viii) x, y, z+1; (ix) x1, y, z1; (x) x+1, y, z+1.

Experimental details

Crystal data
Chemical formulaK3[Pb(C2H3O2)2(NCS)](NCS)2
Mr616.82
Crystal system, space groupMonoclinic, P21/m
Temperature (K)140
a, b, c (Å)6.1968 (1), 19.2499 (3), 7.6354 (1)
β (°) 106.982 (1)
V3)871.10 (2)
Z2
Radiation typeMo Kα
µ (mm1)10.77
Crystal size (mm)0.25 × 0.20 × 0.08
Data collection
DiffractometerBruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.174, 0.480
No. of measured, independent and
observed [I > 2σ(I)] reflections
6058, 2045, 2015
Rint0.023
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.056, 1.16
No. of reflections2045
No. of parameters104
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.81, 2.00

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

 

Acknowledgements

I thank Dr Maryam Ranjbar of the Iranian Research Organization for Science and Technology for providing the crystal, and the University of Malaya for supporting this study.

References

First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS Google Scholar
First citationBruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationMorsali, A. & Mahjoub, A. R. (2004). Helv. Chim. Acta, 87, 2717–2722.  Web of Science CSD CrossRef CAS Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWestrip, S. P. (2009). publCIF. In preparation.  Google Scholar

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