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The asymmetric unit of the title compound, C22H21N3O22+·2I-, consists of a substituted bipyridinium cation and two iodide anions. The dihedral angle between the two rings within the phthal­imide moiety is 1.7 (3)°, where the r.m.s. deviations for the five- and six-membered rings are 0.006 and 0.004 Å, respectively. On the other hand, the two pyridinium rings are tilted at an angle of 3.9 (3)° because of the steric contacts between the H atoms at the 3-, 5-, 3'- and 5'-positions of the 4,4'-bipyridinium moiety. The phthal­imide plane is tilted by 68.5 (1)° with respect to the pyridinium plane, directly attached to the propyl­ene moiety.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803012376/dn6076sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803012376/dn6076Isup2.hkl
Contains datablock I

CCDC reference: 217438

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.041
  • wR factor = 0.102
  • Data-to-parameter ratio = 18.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 4883 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 5280 Completeness (_total/calc) 92.48% Alert C: < 95% complete
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

A photochemical system made up of Ru(bpy)32+ (bpy = 2,2'-bipyridine) and methylviologen (usually, N,N'-dimethyl-4,4'-bipyridinium dichloride) has been thought of as one of the promising candidates to achieve artificial photosynthetic devices. We previously reported that some amidate-bridged platinum dimers with the general formula of [Pt2(NH3)4(µ-amidato)2]2+ (amidate = acetamidate, α-pyrrolidinonate, α-pyridonate, etc.) serve as an effective H2-producing catalyst in a well known photosystem consisting of edta, Ru(bpy)32+ and methylviologen (Sakai et al., 1993). Since then, various efforts have been made to develop a more effective system in which the chemical species mentioned above are linked together to give a single molecular device. The title compound, (I), is obtained as a precursor in such studies.

The molecular structure and the crystal packing diagram for (I) are shown in Figs. 1 and 2, respectively. All bond distances and angles in (I) are observed as expected.

Experimental top

A solution of N-methyl-4,4'-bipyridinium iodide (1.0 mmol; Van Emon et al., 1986) and N-(3-bromopropyl)phthalimide (1.1 mmol) in methanol (20 ml) was refluxed for 2 d. The red prisms or plates deposited were collected by filtration and air-dried (yield: 52%). The purity has been checked by 1H NMR spectroscopy.

Refinement top

All H atoms were located at their idealized positions as riding atoms [C—H(aromatic) = 0.93 Å, CH(methylene) = 0.97 Å and CH(methyl) = 0.96 Å]. In the final difference Fourier synthesis, five residual peaks in the range 1.01–1.27 e Å−3 were observed within 0.94 Å of I atoms.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2002); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997), TEXSAN (Molecular Structure Corporation, 2001), KENX (Sakai, 2002) and ORTEPII (Johnson, 1976).

Figures top
[Figure 1] Fig. 1. The structure of the independent cation and anions in (I), showing the atom-labeling scheme. Displacement ellipsoids are shown at the 50% probability level.
[Figure 2] Fig. 2. Crystal packing view down the a axis of (I).
N-Methyl-N'-(3-phthalimidopropyl)-4,4'-bipyridinium diiodide top
Crystal data top
C22H21N3O22+·2IZ = 2
Mr = 613.22F(000) = 592
Triclinic, P1? # Insert any comments here.
Hall symbol: -P 1Dx = 1.775 Mg m3
a = 6.0535 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 7.4674 (6) ÅCell parameters from 3414 reflections
c = 25.776 (2) Åθ = 2.8–27.2°
α = 83.715 (1)°µ = 2.76 mm1
β = 88.570 (2)°T = 296 K
γ = 82.223 (1)°Plate, red
V = 1147.45 (16) Å30.20 × 0.20 × 0.05 mm
Data collection top
Bruker SMART APEX CCD-detector
diffractometer
4883 independent reflections
Radiation source: fine-focus sealed tube4060 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 8.366 pixels mm-1θmax = 27.5°, θmin = 2.4°
ω scansh = 77
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 89
Tmin = 0.586, Tmax = 0.871l = 2433
6983 measured reflections
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.102H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.048P)2 + 0.5905P]
where P = (Fo2 + 2Fc2)/3
4883 reflections(Δ/σ)max = 0.001
263 parametersΔρmax = 1.27 e Å3
0 restraintsΔρmin = 0.44 e Å3
Crystal data top
C22H21N3O22+·2Iγ = 82.223 (1)°
Mr = 613.22V = 1147.45 (16) Å3
Triclinic, P1Z = 2
a = 6.0535 (5) ÅMo Kα radiation
b = 7.4674 (6) ŵ = 2.76 mm1
c = 25.776 (2) ÅT = 296 K
α = 83.715 (1)°0.20 × 0.20 × 0.05 mm
β = 88.570 (2)°
Data collection top
Bruker SMART APEX CCD-detector
diffractometer
4883 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
4060 reflections with I > 2σ(I)
Tmin = 0.586, Tmax = 0.871Rint = 0.019
6983 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0410 restraints
wR(F2) = 0.102H-atom parameters constrained
S = 1.05Δρmax = 1.27 e Å3
4883 reflectionsΔρmin = 0.44 e Å3
263 parameters
Special details top

Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data.

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.

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

− 3.2752 (0.0107) x − 3.4850 (0.0128) y + 17.5481 (0.0380) z = 5.2837 (0.0195)

* 0.0038 (0.0025) N1 * 0.0018 (0.0025) C1 * −0.0069 (0.0026) C2 * 0.0091 (0.0026) C7 * −0.0077 (0.0024) C8 0.0319 (0.0065) O1 − 0.0086 (0.0065) O2

Rms deviation of fitted atoms = 0.0064

− 3.1971 (0.0099) x − 3.6691 (0.0124) y + 17.3429 (0.0361) z = 5.1130 (0.0218)

Angle to previous plane (with approximate e.s.d.) = 1.72 (0.31)

* −0.0021 (0.0030) C2 * −0.0016 (0.0032) C3 * 0.0056 (0.0034) C4 * −0.0057 (0.0036) C5 * 0.0019 (0.0034) C6 * 0.0019 (0.0030) C7 0.1042 (0.0082) O1 0.0235 (0.0081) O2

Rms deviation of fitted atoms = 0.0036

− 3.2327 (0.0078) x − 3.5891 (0.0060) y + 17.4312 (0.0251) z = 5.2054 (0.0128)

Angle to previous plane (with approximate e.s.d.) = 0.76 (0.26)

* 0.0199 (0.0029) N1 * 0.0107 (0.0032) C1 * −0.0231 (0.0037) C2 * −0.0109 (0.0035) C3 * 0.0142 (0.0038) C4 * 0.0084 (0.0041) C5 * 0.0040 (0.0038) C6 * −0.0135 (0.0037) C7 * −0.0097 (0.0032) C8 0.0534 (0.0055) O1 − 0.0088 (0.0055) O2

Rms deviation of fitted atoms = 0.0138

3.5617 (0.0072) x − 1.9039 (0.0123) y + 18.2690 (0.0275) z = 6.0355 (0.0080)

Angle to previous plane (with approximate e.s.d.) = 68.45 (0.10)

* 0.0053 (0.0025) N2 * 0.0009 (0.0026) C12 * −0.0071 (0.0028) C13 * 0.0073 (0.0026) C14 * −0.0014 (0.0027) C15 * −0.0049 (0.0028) C16

Rms deviation of fitted atoms = 0.0051

3.5183 (0.0076) x − 2.3694 (0.0130) y + 17.4322 (0.0308) z = 5.8040 (0.0118)

Angle to previous plane (with approximate e.s.d.) = 3.87 (1/4)

* −0.0065 (0.0026) N3 * −0.0017 (0.0030) C17 * 0.0093 (0.0030) C18 * −0.0089 (0.0027) C19 * 0.0011 (0.0027) C20 * 0.0067 (0.0027) C21

Rms deviation of fitted atoms = 0.0065

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
xyzUiso*/Ueq
I10.19500 (5)0.72933 (4)0.254201 (15)0.06628 (13)
I20.84565 (5)0.74396 (4)0.065322 (12)0.05327 (11)
O10.4876 (5)0.2479 (5)0.44316 (13)0.0672 (9)
O20.1257 (6)0.3202 (5)0.34073 (14)0.0749 (10)
N10.1978 (6)0.2446 (5)0.38681 (13)0.0492 (8)
N20.5727 (5)0.2105 (4)0.24093 (12)0.0377 (7)
N31.4807 (5)0.2657 (4)0.06983 (12)0.0398 (7)
C10.3138 (7)0.3200 (6)0.42332 (16)0.0499 (10)
C20.1766 (7)0.4947 (6)0.43191 (16)0.0489 (10)
C30.2117 (8)0.6203 (6)0.46498 (18)0.0586 (11)
H30.33900.60640.48530.070*
C40.0484 (10)0.7685 (7)0.4666 (2)0.0697 (14)
H40.06480.85580.48890.084*
C50.1378 (10)0.7887 (8)0.4359 (2)0.0776 (16)
H50.24340.89090.43730.093*
C60.1721 (9)0.6599 (8)0.4028 (2)0.0715 (14)
H60.29900.67270.38240.086*
C70.0104 (7)0.5141 (6)0.40176 (17)0.0527 (10)
C80.0021 (7)0.3550 (7)0.37156 (17)0.0552 (11)
C90.2768 (8)0.0703 (6)0.36789 (16)0.0530 (11)
H9A0.15300.02570.35250.064*
H9B0.32870.01630.39730.064*
C100.4626 (7)0.0793 (5)0.32801 (15)0.0465 (9)
H10A0.58370.13010.34250.056*
H10B0.51910.04270.32010.056*
C110.3849 (6)0.1939 (5)0.27838 (15)0.0434 (9)
H11A0.27030.13910.26260.052*
H11B0.32030.31390.28640.052*
C120.6752 (7)0.3591 (5)0.23621 (15)0.0433 (9)
H120.62500.45380.25600.052*
C130.8524 (6)0.3747 (5)0.20284 (16)0.0420 (9)
H130.92050.47980.19970.050*
C140.9306 (6)0.2327 (5)0.17358 (14)0.0345 (7)
C150.8192 (6)0.0811 (5)0.17903 (15)0.0420 (9)
H150.86590.01540.15970.050*
C160.6415 (7)0.0722 (5)0.21254 (16)0.0453 (9)
H160.56790.03000.21570.054*
C171.3702 (7)0.1209 (6)0.07274 (17)0.0503 (10)
H171.41330.02940.05140.060*
C181.1957 (7)0.1061 (5)0.10658 (17)0.0478 (10)
H181.12240.00370.10860.057*
C191.1264 (6)0.2432 (5)0.13816 (14)0.0361 (8)
C201.2465 (7)0.3901 (5)0.13447 (15)0.0425 (9)
H201.20720.48380.15530.051*
C211.4225 (6)0.3974 (5)0.10025 (15)0.0417 (9)
H211.50250.49580.09830.050*
C221.6680 (7)0.2759 (6)0.03166 (17)0.0495 (10)
H22A1.60970.30050.00310.074*
H22B1.76450.16220.03470.074*
H22C1.75060.37140.03870.074*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.0654 (2)0.03703 (17)0.1002 (3)0.01153 (14)0.01225 (18)0.01576 (15)
I20.05358 (18)0.03899 (16)0.0708 (2)0.01621 (12)0.00222 (14)0.00893 (13)
O10.062 (2)0.074 (2)0.066 (2)0.0056 (17)0.0165 (17)0.0240 (17)
O20.066 (2)0.090 (3)0.075 (2)0.0285 (19)0.0166 (18)0.0111 (19)
N10.052 (2)0.056 (2)0.0440 (19)0.0184 (17)0.0002 (16)0.0115 (16)
N20.0386 (16)0.0334 (16)0.0407 (17)0.0050 (13)0.0008 (13)0.0016 (13)
N30.0373 (16)0.0357 (16)0.0467 (18)0.0064 (13)0.0003 (14)0.0041 (13)
C10.054 (2)0.058 (3)0.041 (2)0.014 (2)0.0009 (19)0.0103 (18)
C20.053 (2)0.051 (2)0.043 (2)0.0112 (19)0.0062 (19)0.0053 (18)
C30.068 (3)0.054 (3)0.055 (3)0.009 (2)0.003 (2)0.010 (2)
C40.094 (4)0.051 (3)0.063 (3)0.009 (3)0.011 (3)0.007 (2)
C50.081 (4)0.064 (3)0.080 (4)0.006 (3)0.019 (3)0.004 (3)
C60.062 (3)0.081 (4)0.065 (3)0.003 (3)0.002 (2)0.011 (3)
C70.051 (2)0.057 (3)0.050 (2)0.011 (2)0.0036 (19)0.002 (2)
C80.052 (3)0.070 (3)0.047 (2)0.025 (2)0.000 (2)0.001 (2)
C90.068 (3)0.052 (2)0.044 (2)0.026 (2)0.001 (2)0.0043 (18)
C100.052 (2)0.041 (2)0.049 (2)0.0124 (18)0.0018 (19)0.0051 (17)
C110.043 (2)0.040 (2)0.048 (2)0.0071 (17)0.0019 (17)0.0038 (16)
C120.049 (2)0.037 (2)0.045 (2)0.0068 (17)0.0011 (18)0.0115 (16)
C130.042 (2)0.0325 (18)0.055 (2)0.0131 (16)0.0019 (17)0.0110 (16)
C140.0359 (18)0.0293 (17)0.0384 (19)0.0046 (14)0.0029 (15)0.0033 (14)
C150.046 (2)0.0301 (18)0.050 (2)0.0065 (16)0.0041 (18)0.0079 (16)
C160.054 (2)0.0302 (18)0.053 (2)0.0114 (17)0.0057 (19)0.0052 (16)
C170.047 (2)0.045 (2)0.065 (3)0.0169 (18)0.009 (2)0.0222 (19)
C180.049 (2)0.039 (2)0.062 (3)0.0173 (18)0.007 (2)0.0207 (18)
C190.0368 (18)0.0293 (17)0.042 (2)0.0052 (14)0.0060 (15)0.0023 (14)
C200.051 (2)0.0305 (18)0.048 (2)0.0105 (16)0.0002 (18)0.0067 (15)
C210.046 (2)0.0293 (18)0.051 (2)0.0118 (16)0.0008 (18)0.0027 (16)
C220.045 (2)0.048 (2)0.057 (3)0.0128 (18)0.0096 (19)0.0081 (19)
Geometric parameters (Å, º) top
O1—C11.213 (5)C10—C111.507 (5)
O2—C81.195 (5)C10—H10A0.9700
N1—C81.387 (6)C10—H10B0.9700
N1—C11.397 (5)C11—H11A0.9700
N1—C91.456 (5)C11—H11B0.9700
N2—C121.336 (5)C12—C131.367 (5)
N2—C161.345 (5)C12—H120.9300
N2—C111.482 (5)C13—C141.392 (5)
N3—C211.329 (5)C13—H130.9300
N3—C171.341 (5)C14—C151.386 (5)
N3—C221.486 (5)C14—C191.483 (5)
C1—C21.483 (6)C15—C161.367 (5)
C2—C71.372 (6)C15—H150.9300
C2—C31.375 (6)C16—H160.9300
C3—C41.384 (7)C17—C181.362 (6)
C3—H30.9300C17—H170.9300
C4—C51.375 (8)C18—C191.392 (5)
C4—H40.9300C18—H180.9300
C5—C61.393 (8)C19—C201.389 (5)
C5—H50.9300C20—C211.369 (5)
C6—C71.364 (7)C20—H200.9300
C6—H60.9300C21—H210.9300
C7—C81.483 (6)C22—H22A0.9600
C9—C101.508 (5)C22—H22B0.9600
C9—H9A0.9700C22—H22C0.9600
C9—H9B0.9700
C8—N1—C1111.9 (4)H10A—C10—H10B107.9
C8—N1—C9125.2 (4)N2—C11—C10110.9 (3)
C1—N1—C9122.9 (4)N2—C11—H11A109.5
C12—N2—C16120.5 (3)C10—C11—H11A109.5
C12—N2—C11120.5 (3)N2—C11—H11B109.5
C16—N2—C11119.1 (3)C10—C11—H11B109.5
C21—N3—C17120.5 (3)H11A—C11—H11B108.0
C21—N3—C22121.0 (3)N2—C12—C13121.2 (3)
C17—N3—C22118.5 (3)N2—C12—H12119.4
O1—C1—N1124.3 (4)C13—C12—H12119.4
O1—C1—C2130.2 (4)C12—C13—C14119.8 (3)
N1—C1—C2105.5 (4)C12—C13—H13120.1
C7—C2—C3122.1 (5)C14—C13—H13120.1
C7—C2—C1108.4 (4)C15—C14—C13117.5 (3)
C3—C2—C1129.5 (4)C15—C14—C19121.4 (3)
C2—C3—C4116.8 (5)C13—C14—C19121.1 (3)
C2—C3—H3121.6C16—C15—C14120.7 (3)
C4—C3—H3121.6C16—C15—H15119.7
C5—C4—C3121.0 (5)C14—C15—H15119.7
C5—C4—H4119.5N2—C16—C15120.3 (3)
C3—C4—H4119.5N2—C16—H16119.8
C4—C5—C6121.6 (5)C15—C16—H16119.8
C4—C5—H5119.2N3—C17—C18120.9 (4)
C6—C5—H5119.2N3—C17—H17119.6
C7—C6—C5116.7 (5)C18—C17—H17119.6
C7—C6—H6121.7C17—C18—C19120.3 (4)
C5—C6—H6121.7C17—C18—H18119.8
C6—C7—C2121.8 (5)C19—C18—H18119.8
C6—C7—C8129.9 (5)C20—C19—C18117.2 (3)
C2—C7—C8108.3 (4)C20—C19—C14121.9 (3)
O2—C8—N1124.5 (5)C18—C19—C14120.9 (3)
O2—C8—C7129.6 (5)C21—C20—C19120.2 (4)
N1—C8—C7105.8 (4)C21—C20—H20119.9
N1—C9—C10113.5 (3)C19—C20—H20119.9
N1—C9—H9A108.9N3—C21—C20121.0 (3)
C10—C9—H9A108.9N3—C21—H21119.5
N1—C9—H9B108.9C20—C21—H21119.5
C10—C9—H9B108.9N3—C22—H22A109.5
H9A—C9—H9B107.7N3—C22—H22B109.5
C11—C10—C9111.7 (3)H22A—C22—H22B109.5
C11—C10—H10A109.3N3—C22—H22C109.5
C9—C10—H10A109.3H22A—C22—H22C109.5
C11—C10—H10B109.3H22B—C22—H22C109.5
C9—C10—H10B109.3
C8—N1—C1—O1178.8 (4)N1—C9—C10—C1165.6 (5)
C9—N1—C1—O11.1 (7)C12—N2—C11—C1099.4 (4)
C8—N1—C1—C20.2 (5)C16—N2—C11—C1079.2 (4)
C9—N1—C1—C2179.6 (3)C9—C10—C11—N2176.5 (3)
O1—C1—C2—C7177.6 (5)C16—N2—C12—C130.3 (6)
N1—C1—C2—C70.8 (5)C11—N2—C12—C13178.3 (4)
O1—C1—C2—C30.2 (8)N2—C12—C13—C140.8 (6)
N1—C1—C2—C3178.2 (4)C12—C13—C14—C151.4 (6)
C7—C2—C3—C40.1 (7)C12—C13—C14—C19178.3 (4)
C1—C2—C3—C4177.0 (4)C13—C14—C15—C160.9 (6)
C2—C3—C4—C50.9 (7)C19—C14—C15—C16178.8 (4)
C3—C4—C5—C61.3 (8)C12—N2—C16—C150.9 (6)
C4—C5—C6—C70.9 (8)C11—N2—C16—C15177.8 (4)
C5—C6—C7—C20.2 (7)C14—C15—C16—N20.3 (6)
C5—C6—C7—C8179.4 (4)C21—N3—C17—C180.4 (6)
C3—C2—C7—C60.2 (7)C22—N3—C17—C18179.2 (4)
C1—C2—C7—C6177.9 (4)N3—C17—C18—C191.2 (7)
C3—C2—C7—C8179.1 (4)C17—C18—C19—C201.8 (6)
C1—C2—C7—C81.5 (5)C17—C18—C19—C14177.4 (4)
C1—N1—C8—O2180.0 (4)C15—C14—C19—C20176.5 (3)
C9—N1—C8—O20.2 (7)C13—C14—C19—C203.2 (6)
C1—N1—C8—C71.1 (5)C15—C14—C19—C184.3 (6)
C9—N1—C8—C7178.7 (3)C13—C14—C19—C18176.0 (4)
C6—C7—C8—O21.1 (8)C18—C19—C20—C211.0 (6)
C2—C7—C8—O2179.6 (5)C14—C19—C20—C21178.2 (4)
C6—C7—C8—N1177.7 (4)C17—N3—C21—C201.2 (6)
C2—C7—C8—N11.6 (5)C22—N3—C21—C20178.3 (4)
C8—N1—C9—C10103.0 (5)C19—C20—C21—N30.5 (6)
C1—N1—C9—C1077.2 (5)

Experimental details

Crystal data
Chemical formulaC22H21N3O22+·2I
Mr613.22
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)6.0535 (5), 7.4674 (6), 25.776 (2)
α, β, γ (°)83.715 (1), 88.570 (2), 82.223 (1)
V3)1147.45 (16)
Z2
Radiation typeMo Kα
µ (mm1)2.76
Crystal size (mm)0.20 × 0.20 × 0.05
Data collection
DiffractometerBruker SMART APEX CCD-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.586, 0.871
No. of measured, independent and
observed [I > 2σ(I)] reflections
6983, 4883, 4060
Rint0.019
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.102, 1.05
No. of reflections4883
No. of parameters263
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.27, 0.44

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), TEXSAN (Molecular Structure Corporation, 2001), KENX (Sakai, 2002) and ORTEPII (Johnson, 1976).

 

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