μ-Oxido-bis­{chlorido[tris­(2-pyridylmeth­yl)amine]chromium(III)} bis(hexafluoridophosphate)

Li, S.; Wang, S.-B.; Zhang, F.-L.; Tang, K.

doi:10.1107/S1600536807061296

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 1| January 2008| Page m2

https://doi.org/10.1107/S1600536807061296

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RETRACTED ARTICLE

This article has been retracted. To view the retraction notice, click here.

Retracted: μ-Oxido-bis{chlorido[tris(2-pyridylmethyl)amine]chromium(III)} bis(hexafluoridophosphate)

Sheng Li,^a ^* Shou-Bin Wang,^b Fu-Li Zhang ^a and Kun Tang ^a

^aCollege of Medicine, Henan University, Kaifeng 475003, People's Republic of China, and ^bCollege of Chemistry and Chemical Engineering, Henan University, Kaifeng 475003, People's Republic of China
^*Correspondence e-mail: lisheng0821@sina.com

(Received 22 October 2007; accepted 20 November 2007; online 6 December 2007)

The title compound, [Cr₂Cl₂O(C₁₈H₁₈N₄)₂](PF₆)₂, is isostructural with the V^III analogue. Each Cr^III atom is chelated by the tetradentate tris(2-pyridylmethyl)amine ligand via four N atoms, and further coordinated by one Cl atom and one bridging O atom, giving a slightly distorted octahedral coordination geometry. The dinuclear complex is centrosymmetric, with the bridging O atom lying on a centre of inversion.

Related literature

For the isostructural V^III analogue, see: Tajika et al. (2005 ). For more general related literature, see: Butler & Carrano (1991 ); Crans et al. (1989 ); Dey (1974 ); Chen & Zubieta (1990 ).

Experimental

Crystal data

[Cr₂Cl₂O(C₁₈H₁₈N₄)₂](PF₆)₂
M_r = 1061.57
Triclinic, $[P \overline 1]$
a = 8.6107 (17) Å
b = 11.302 (2) Å
c = 12.798 (3) Å
α = 115.50 (3)°
β = 107.45 (3)°
γ = 91.50 (3)°
V = 1054.8 (4) Å³
Z = 1
Mo Kα radiation
μ = 0.81 mm⁻¹
T = 293 (2) K
0.28 × 0.22 × 0.18 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ) T_min = 0.804, T_max = 0.867
8686 measured reflections
3877 independent reflections
3594 reflections with I > 2σ(I)
R_int = 0.021

Refinement

R[F² > 2σ(F²)] = 0.033
wR(F²) = 0.089
S = 1.00
3877 reflections
287 parameters
H-atom parameters constrained
Δρ_max = 0.51 e Å⁻³
Δρ_min = −0.33 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536807061296/bi2257sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807061296/bi2257Isup2.hkl

checkCIF report

Comment top

A classical but nevertheless rapidly developing field of application for related metal-Schiff compounds is their use as catalysts in polymerization, oxidation reactions, and model examples for the interaction of metal ions within the active sites of enzymes (Butler & Carrano, 1991; Crans et al., 1989; Dey, 1974; Chen & Zubieta, 1990). In the dinuclear title compound (Fig. 1), each Cr^III atom is chelated by the tetradentate ligand tris(2-pyridylmethyl)amine via four N atoms, and further coordinated by one Cl atom and one bridging O atom to give a slightly distorted octahedral coordination geometry.

Related literature top

For the isostructural V^III analogue, see: Tajika et al. (2005). For more general related literature, see: Butler & Carrano (1991); Crans et al. (1989); Dey (1974); Chen & Zubieta (1990).

Experimental top

A mixture of chromium(III) trichloride (1 mmol) and tris(2-pyridylmethyl)amine (1 mmol) in 20 ml me thanol was refluxed for two hours. After cooling, the solution was filtered and the filtrate was evaporated naturally at room temperature. Blue blocks of the title compound were obtained after a few days with a yield of 31%. Elemental analysis calculated: C 40.39, H 3.35, N 10.44%; found: C 40.35, H 3.39, N 10.42%.

Structure description top

For the isostructural V^III analogue, see: Tajika et al. (2005). For more general related literature, see: Butler & Carrano (1991); Crans et al. (1989); Dey (1974); Chen & Zubieta (1990).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).

Figures top

Fig. 1. The molecular structure drawn with 30% probability displacement ellipsoids for the non-H atoms.

µ-Oxido-bis{chlorido[tris(2-pyridylmethyl)amine]chromium(III)} dihexafluoridophosphate top

Crystal data top

[Cr₂Cl₂O(C₁₈H₁₈N₄)₂](PF₆)₂	Z = 1
M_r = 1061.57	F(000) = 536
Triclinic, P1	D_x = 1.671 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.6107 (17) Å	Cell parameters from 3877 reflections
b = 11.302 (2) Å	θ = 3.0–25.5°
c = 12.798 (3) Å	µ = 0.81 mm⁻¹
α = 115.50 (3)°	T = 293 K
β = 107.45 (3)°	Block, blue
γ = 91.50 (3)°	0.28 × 0.22 × 0.18 mm
V = 1054.8 (4) Å³

Data collection top

Bruker APEX II CCD diffractometer	3877 independent reflections
Radiation source: fine-focus sealed tube	3594 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
φ and ω scans	θ_max = 25.5°, θ_min = 3.0°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −8→10
T_min = 0.804, T_max = 0.867	k = −13→13
8686 measured reflections	l = −15→15

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)] = 0.033	H-atom parameters constrained
wR(F²) = 0.089	w = 1/[σ²(F_o²) + (0.0565P)² + 0.3428P] where P = (F_o² + 2F_c²)/3
S = 1.00	(Δ/σ)_max < 0.001
3877 reflections	Δρ_max = 0.51 e Å⁻³
287 parameters	Δρ_min = −0.33 e Å⁻³
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.042 (3)

Crystal data top

[Cr₂Cl₂O(C₁₈H₁₈N₄)₂](PF₆)₂	γ = 91.50 (3)°
M_r = 1061.57	V = 1054.8 (4) Å³
Triclinic, P1	Z = 1
a = 8.6107 (17) Å	Mo Kα radiation
b = 11.302 (2) Å	µ = 0.81 mm⁻¹
c = 12.798 (3) Å	T = 293 K
α = 115.50 (3)°	0.28 × 0.22 × 0.18 mm
β = 107.45 (3)°

Data collection top

Bruker APEX II CCD diffractometer	3877 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2001)	3594 reflections with I > 2σ(I)
T_min = 0.804, T_max = 0.867	R_int = 0.021
8686 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.033	0 restraints
wR(F²) = 0.089	H-atom parameters constrained
S = 1.00	Δρ_max = 0.51 e Å⁻³
3877 reflections	Δρ_min = −0.33 e Å⁻³
287 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
Cr1	1.03745 (3)	0.34679 (3)	0.39271 (2)	0.0408 (4)
C1	0.9871 (3)	0.1897 (2)	0.53070 (18)	0.0447 (4)
H1	1.1018	0.1984	0.5573	0.054*
C2	0.8992 (3)	0.1306 (2)	0.5741 (2)	0.0534 (5)
H2	0.9533	0.0998	0.6296	0.064*
C3	0.7284 (3)	0.1173 (3)	0.5340 (2)	0.0605 (6)
H3	0.6662	0.0779	0.5626	0.073*
C4	0.6514 (3)	0.1630 (2)	0.4513 (2)	0.0552 (5)
H4	0.5367	0.1537	0.4226	0.066*
C5	0.7464 (2)	0.22306 (19)	0.41135 (18)	0.0425 (4)
C6	0.6721 (2)	0.2874 (2)	0.3310 (2)	0.0490 (5)
H6A	0.5643	0.2353	0.2730	0.059*
H6B	0.6563	0.3757	0.3822	0.059*
C7	0.7467 (3)	0.1753 (2)	0.1450 (2)	0.0573 (6)
H7A	0.7443	0.2004	0.0811	0.069*
H7B	0.6381	0.1253	0.1216	0.069*
C8	0.8712 (2)	0.08565 (19)	0.14924 (17)	0.0414 (4)
C9	0.8351 (3)	−0.0448 (2)	0.0588 (2)	0.0528 (5)
H9	0.7315	−0.0793	−0.0028	0.063*
C10	0.9546 (3)	−0.1237 (2)	0.0606 (2)	0.0617 (6)
H10	0.9327	−0.2119	0.0003	0.074*
C11	1.1069 (3)	−0.0697 (2)	0.1532 (2)	0.0607 (6)
H11	1.1894	−0.1208	0.1564	0.073*
C12	1.1346 (3)	0.0605 (2)	0.2404 (2)	0.0526 (5)
H12	1.2374	0.0964	0.3028	0.063*
C13	0.7605 (3)	0.4147 (2)	0.23723 (19)	0.0475 (5)
H13A	0.7430	0.4881	0.3059	0.057*
H13B	0.6651	0.3917	0.1639	0.057*
C14	0.9146 (3)	0.4574 (2)	0.21891 (17)	0.0471 (5)
C15	0.9138 (4)	0.5296 (2)	0.1547 (2)	0.0606 (6)
H15	0.8154	0.5482	0.1149	0.073*
C16	1.0629 (4)	0.5734 (3)	0.1512 (2)	0.0728 (8)
H16	1.0650	0.6237	0.1100	0.087*
C17	1.2075 (4)	0.5435 (3)	0.2077 (3)	0.0715 (7)
H17	1.3076	0.5721	0.2047	0.086*
C18	1.2007 (3)	0.4704 (3)	0.2686 (2)	0.0610 (6)
H18	1.2978	0.4490	0.3069	0.073*
Cl1	1.31398 (6)	0.35078 (6)	0.48445 (5)	0.05507 (17)
F1	0.5115 (2)	0.90789 (16)	0.13882 (17)	0.0825 (5)
F2	0.4878 (2)	0.8490 (2)	0.27945 (15)	0.0893 (5)
F3	0.5830 (3)	0.6607 (2)	0.1912 (2)	0.1078 (7)
F4	0.7325 (2)	0.8610 (2)	0.24906 (17)	0.0999 (6)
F5	0.6040 (2)	0.72005 (19)	0.04870 (17)	0.0929 (6)
F6	0.36012 (19)	0.71102 (16)	0.08031 (14)	0.0726 (4)
N1	1.0192 (2)	0.13917 (16)	0.23969 (15)	0.0436 (4)
N2	1.0566 (2)	0.42848 (18)	0.27454 (16)	0.0482 (4)
N3	0.91312 (19)	0.23567 (15)	0.45104 (15)	0.0406 (3)
N4	0.7776 (2)	0.29834 (16)	0.26214 (15)	0.0424 (4)
O1	1.0000	0.5000	0.5000	0.0420 (4)
P1	0.54870 (7)	0.78424 (6)	0.16549 (5)	0.05276 (17)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.0378 (11)	0.0424 (10)	0.0424 (10)	0.0088 (8)	0.0112 (8)	0.0212 (8)
C1	0.0415 (10)	0.0468 (10)	0.0459 (10)	0.0095 (8)	0.0121 (8)	0.0233 (8)
C2	0.0597 (14)	0.0546 (12)	0.0513 (12)	0.0109 (10)	0.0179 (10)	0.0300 (10)
C3	0.0606 (14)	0.0666 (14)	0.0669 (14)	0.0057 (11)	0.0281 (11)	0.0381 (12)
C4	0.0395 (11)	0.0606 (13)	0.0695 (14)	0.0063 (9)	0.0206 (10)	0.0324 (11)
C5	0.0351 (9)	0.0412 (9)	0.0456 (10)	0.0057 (7)	0.0117 (8)	0.0166 (8)
C6	0.0302 (9)	0.0572 (12)	0.0614 (12)	0.0093 (8)	0.0107 (8)	0.0322 (10)
C7	0.0517 (13)	0.0499 (12)	0.0462 (11)	0.0099 (9)	−0.0011 (9)	0.0127 (9)
C8	0.0424 (10)	0.0438 (10)	0.0403 (9)	0.0052 (8)	0.0153 (8)	0.0207 (8)
C9	0.0562 (13)	0.0484 (11)	0.0497 (11)	0.0027 (9)	0.0185 (10)	0.0189 (9)
C10	0.0769 (17)	0.0441 (11)	0.0634 (14)	0.0138 (11)	0.0334 (13)	0.0178 (10)
C11	0.0653 (15)	0.0551 (13)	0.0714 (15)	0.0256 (11)	0.0342 (12)	0.0297 (11)
C12	0.0460 (12)	0.0572 (12)	0.0570 (12)	0.0167 (9)	0.0199 (10)	0.0265 (10)
C13	0.0504 (11)	0.0490 (11)	0.0410 (10)	0.0162 (9)	0.0097 (8)	0.0224 (9)
C14	0.0599 (13)	0.0426 (10)	0.0358 (9)	0.0112 (9)	0.0152 (9)	0.0162 (8)
C15	0.0864 (18)	0.0503 (12)	0.0451 (12)	0.0140 (11)	0.0197 (11)	0.0237 (10)
C16	0.114 (2)	0.0544 (13)	0.0572 (14)	0.0012 (14)	0.0362 (15)	0.0288 (12)
C17	0.084 (2)	0.0710 (16)	0.0683 (16)	−0.0005 (14)	0.0357 (14)	0.0343 (13)
C18	0.0612 (14)	0.0666 (14)	0.0615 (14)	0.0042 (11)	0.0280 (11)	0.0307 (12)
Cl1	0.0334 (3)	0.0609 (3)	0.0596 (3)	0.0131 (2)	0.0101 (2)	0.0215 (2)
F1	0.0810 (11)	0.0724 (10)	0.0988 (12)	0.0060 (8)	0.0208 (9)	0.0507 (9)
F2	0.0836 (12)	0.1141 (14)	0.0632 (9)	0.0059 (10)	0.0336 (8)	0.0300 (9)
F3	0.1008 (15)	0.1236 (16)	0.163 (2)	0.0524 (12)	0.0641 (14)	0.1074 (16)
F4	0.0483 (9)	0.1549 (19)	0.0854 (12)	−0.0063 (10)	0.0024 (8)	0.0605 (12)
F5	0.0973 (13)	0.0965 (12)	0.0873 (12)	0.0083 (10)	0.0563 (10)	0.0288 (10)
F6	0.0571 (9)	0.0710 (9)	0.0731 (9)	−0.0042 (7)	0.0144 (7)	0.0248 (7)
N1	0.0425 (9)	0.0456 (9)	0.0444 (9)	0.0116 (7)	0.0164 (7)	0.0210 (7)
N2	0.0526 (10)	0.0497 (9)	0.0451 (9)	0.0087 (8)	0.0187 (8)	0.0231 (8)
N3	0.0348 (8)	0.0421 (8)	0.0447 (8)	0.0082 (6)	0.0125 (7)	0.0205 (7)
N4	0.0376 (8)	0.0442 (8)	0.0411 (8)	0.0101 (7)	0.0077 (6)	0.0195 (7)
O1	0.0384 (10)	0.0430 (10)	0.0424 (10)	0.0081 (8)	0.0119 (8)	0.0190 (8)
P1	0.0429 (3)	0.0665 (4)	0.0529 (3)	0.0075 (3)	0.0151 (2)	0.0321 (3)

Geometric parameters (Å, º) top

Cr1—O1	1.7986 (7)	C9—H9	0.930
Cr1—N3	2.1206 (18)	C10—C11	1.378 (4)
Cr1—N2	2.1238 (18)	C10—H10	0.930
Cr1—N4	2.2370 (19)	C11—C12	1.370 (3)
Cr1—N1	2.2814 (19)	C11—H11	0.930
Cr1—Cl1	2.3070 (9)	C12—N1	1.351 (3)
O1—Cr1ⁱ	1.7986 (7)	C12—H12	0.930
C1—N3	1.341 (3)	C13—N4	1.482 (3)
C1—C2	1.369 (3)	C13—C14	1.516 (3)
C1—H1	0.930	C13—H13A	0.970
C2—C3	1.386 (4)	C13—H13B	0.970
C2—H2	0.930	C14—N2	1.345 (3)
C3—C4	1.376 (4)	C14—C15	1.383 (3)
C3—H3	0.930	C15—C16	1.384 (4)
C4—C5	1.382 (3)	C15—H15	0.930
C4—H4	0.930	C16—C17	1.371 (4)
C5—N3	1.352 (3)	C16—H16	0.930
C5—C6	1.506 (3)	C17—C18	1.369 (4)
C6—N4	1.479 (3)	C17—H17	0.930
C6—H6A	0.970	C18—N2	1.351 (3)
C6—H6B	0.970	C18—H18	0.930
C7—N4	1.483 (3)	F1—P1	1.5939 (17)
C7—C8	1.499 (3)	F2—P1	1.5803 (18)
C7—H7A	0.970	F3—P1	1.582 (2)
C7—H7B	0.970	F4—P1	1.5859 (18)
C8—N1	1.342 (3)	F5—P1	1.5804 (18)
C8—C9	1.379 (3)	F6—P1	1.6129 (17)
C9—C10	1.380 (4)

O1—Cr1—N3	91.01 (5)	N1—C12—H12	118.5
O1—Cr1—N2	92.46 (5)	C11—C12—H12	118.5
N3—Cr1—N2	154.67 (7)	N4—C13—C14	110.48 (16)
O1—Cr1—N4	91.36 (6)	N4—C13—H13A	109.6
N3—Cr1—N4	78.03 (7)	C14—C13—H13A	109.6
N2—Cr1—N4	76.81 (7)	N4—C13—H13B	109.6
O1—Cr1—N1	166.58 (5)	C14—C13—H13B	109.6
N3—Cr1—N1	81.87 (7)	H13A—C13—H13B	108.1
N2—Cr1—N1	89.30 (7)	N2—C14—C15	120.7 (2)
N4—Cr1—N1	76.09 (7)	N2—C14—C13	116.67 (18)
O1—Cr1—Cl1	103.29 (5)	C15—C14—C13	122.5 (2)
N3—Cr1—Cl1	104.03 (5)	C14—C15—C16	118.4 (3)
N2—Cr1—Cl1	99.56 (6)	C14—C15—H15	120.8
N4—Cr1—Cl1	165.11 (5)	C16—C15—H15	120.8
N1—Cr1—Cl1	89.52 (6)	C17—C16—C15	120.8 (2)
N3—C1—C2	122.1 (2)	C17—C16—H16	119.6
N3—C1—H1	118.9	C15—C16—H16	119.6
C2—C1—H1	119.0	C16—C17—C18	118.2 (3)
C3—C2—C1	118.8 (2)	C16—C17—H17	120.9
C3—C2—H2	120.6	C18—C17—H17	120.9
C1—C2—H2	120.6	N2—C18—C17	121.8 (3)
C2—C3—C4	119.4 (2)	N2—C18—H18	119.1
C2—C3—H3	120.3	C17—C18—H18	119.1
C4—C3—H3	120.3	C12—N1—C8	117.79 (18)
C3—C4—C5	119.3 (2)	C12—N1—Cr1	126.02 (15)
C3—C4—H4	120.4	C8—N1—Cr1	115.61 (13)
C5—C4—H4	120.4	C14—N2—C18	120.1 (2)
N3—C5—C4	120.95 (19)	C14—N2—Cr1	114.45 (14)
N3—C5—C6	116.79 (18)	C18—N2—Cr1	124.62 (17)
C4—C5—C6	122.07 (19)	C1—N3—C5	119.42 (18)
N4—C6—C5	112.19 (16)	C1—N3—Cr1	125.22 (14)
N4—C6—H6A	109.2	C5—N3—Cr1	115.07 (13)
C5—C6—H6A	109.2	C6—N4—C7	112.30 (18)
N4—C6—H6B	109.2	C6—N4—C13	112.63 (16)
C5—C6—H6B	109.2	C7—N4—C13	109.74 (17)
H6A—C6—H6B	107.9	C6—N4—Cr1	105.11 (12)
N4—C7—C8	114.97 (17)	C7—N4—Cr1	112.78 (13)
N4—C7—H7A	108.5	C13—N4—Cr1	103.96 (12)
C8—C7—H7A	108.5	Cr1—O1—Cr1ⁱ	180.0
N4—C7—H7B	108.5	F5—P1—F3	90.59 (12)
C8—C7—H7B	108.5	F5—P1—F2	178.06 (11)
H7A—C7—H7B	107.5	F3—P1—F2	90.59 (13)
N1—C8—C9	122.2 (2)	F5—P1—F4	90.15 (11)
N1—C8—C7	117.57 (17)	F3—P1—F4	91.62 (13)
C9—C8—C7	120.13 (19)	F2—P1—F4	91.35 (11)
C10—C9—C8	119.3 (2)	F5—P1—F1	89.58 (11)
C10—C9—H9	120.4	F3—P1—F1	179.22 (11)
C8—C9—H9	120.4	F2—P1—F1	89.22 (11)
C11—C10—C9	118.9 (2)	F4—P1—F1	89.14 (11)
C11—C10—H10	120.5	F5—P1—F6	90.19 (10)
C9—C10—H10	120.5	F3—P1—F6	90.39 (12)
C10—C11—C12	118.9 (2)	F2—P1—F6	88.26 (10)
C10—C11—H11	120.6	F4—P1—F6	177.95 (11)
C12—C11—H11	120.6	F1—P1—F6	88.85 (10)
N1—C12—C11	122.9 (2)

Symmetry code: (i) −x+2, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Cr₂Cl₂O(C₁₈H₁₈N₄)₂](PF₆)₂
M_r	1061.57
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	8.6107 (17), 11.302 (2), 12.798 (3)
α, β, γ (°)	115.50 (3), 107.45 (3), 91.50 (3)
V (Å³)	1054.8 (4)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	0.81
Crystal size (mm)	0.28 × 0.22 × 0.18

Data collection
Diffractometer	Bruker APEX II CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.804, 0.867
No. of measured, independent and observed [I > 2σ(I)] reflections	8686, 3877, 3594
R_int	0.021
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.033, 0.089, 1.00
No. of reflections	3877
No. of parameters	287
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.51, −0.33

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001).

Acknowledgements

The authors are grateful for financial support from Henan University (grant No.05YBGG013).

References

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