Poly[μ2-chlorido-dichlorido[μ2-4′-(4-pyrid­yl)-2,2′:6′,2′′-terpyridine]­copper(I)copper(II)]

Zhu, C.-Y.

doi:10.1107/S1600536811014759

metal-organic compounds

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Volume 67| Part 5| May 2011| Page m639

doi:10.1107/S1600536811014759

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Poly[μ₂-chlorido-dichlorido[μ₂-4′-(4-pyridyl)-2,2′:6′,2′′-terpyridine]copper(I)copper(II)]

Chao-Ying Zhu ^a ^*

^aDepartment of Applied Chemistry, Zhejiang Sci-Tech University, Hangzhou 310018, People's Republic of China, and Key Laboratory of Advanced Textile Materials and Manufacturing Technology, Ministry of Education, Zhejiang Sci-Tech University, Hangzhou 310018, People's Republic of China
^*Correspondence e-mail: zstu_zhuchaoying@126.com

(Received 29 March 2011; accepted 20 April 2011; online 29 April 2011)

In the mixed-valence Cu^I/Cu^II coordination polymer, [Cu₂Cl₃(C₂₀H₁₄N₄)]_n, the two Cu atoms are bridged to a pair of Cl atoms across a centre of inversion. The monovalent metal atoms is coordinated by a pyridine N atom as well as by three Cl atoms in a tetrahedral CuNCl₃ geometry. The divalent metal atom is N,N′,N′′-chelated by the heterocycle, and it exists in a square-pyramidal CuN₃Cl₂ geometry; the apical site is occupied by the second bridging Cl atom. The bridging modes of the Cl atoms and the heterocycle give rise to the formation of a layered arrangement parallel to (001).

Related literature

For related structures, see: Hou et al. (2005 ); Zhang et al. (2007 )

Experimental

Crystal data

[Cu₂Cl₃(C₂₀H₁₄N₄)]
M_r = 543.78
Triclinic, $[P \overline 1]$
a = 8.1389 (8) Å
b = 9.8161 (10) Å
c = 12.4823 (13) Å
α = 79.512 (2)°
β = 85.036 (2)°
γ = 88.202 (2)°
V = 976.78 (17) Å³
Z = 2
Mo Kα radiation
μ = 2.60 mm⁻¹
T = 294 K
0.15 × 0.12 × 0.10 mm

Data collection

Bruker SMART diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.694, T_max = 0.771
7840 measured reflections
3778 independent reflections
3391 reflections with I > 2σ(I)
R_int = 0.014

Refinement

R[F² > 2σ(F²)] = 0.027
wR(F²) = 0.072
S = 1.06
3778 reflections
262 parameters
H-atom parameters constrained
Δρ_max = 0.40 e Å⁻³
Δρ_min = −0.34 e Å⁻³

Data collection: SMART (Bruker, 1998 ); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811014759/ng5143sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811014759/ng5143Isup2.hkl

checkCIF report

Comment top

Terpyridine and its derivatives have been receiving rapidly increasing attention recently not only because of their versatility as building blocks in supramolecular assembles, but also due to the interesting electronic, photonic and magnetic properties of their transition metal complexes.

4'-(4-Pyridyl)-2,2':6'2''-terpyridine(pyterpy) belongs to this group of ligands and has usually been used to construct a great variety of structurally interesting entities, such as ribbon-type coordination polymers (Hou et al., 2005) and self-catenated networks (Zhang et al., 2007).

The structure of the title compound (I) is shown in Fig. 1. Single-crystal X-ray diffraction shows that the asymmetric unit contains two Cu crystallographically nonequivalent atoms. The Cu1 atom has a distorted square-pyramidal coordination formed by three N atoms of tridentate 4'-(4-pyridyl)-2,2':6'2''-terpyridine (pyterpy) ligand and two Cl atoms. The Cu2 atom is coordinated by one N atom from the pendent monodentate pyridine of pyterpy as well as by three Cl atoms, conferring a tetrahedral coordination geometry. The two terpy ligands in a transoid arrangement link Cu1 and Cu2 atoms, to form a mixed-valence tetrameric M₄L₄ rectangular unit with a separation of 11.017 Å, which is smaller than those in reported ribbon-type compounds, and then linked by a Cu₂Cl₂ cluster, leading to the formation of an infinite 1-D coordination polymer (Fig. 2).

Related literature top

For related structures, see: Hou et al. (2005); Zhang et al. (2007)

Experimental top

The mixture of CuCl (0.020 g, 0.2 mmol), 4'-(4-pyridyl)-2,2':6'2''-terpyridine (pyterpy) (0.062 g, 0.1 mmol), and acetonitrile (6 ml) were placed and sealed in a 15 ml Teflon-lined stainless steel reactor and heated to 180 °C for 72 h, then cooled down to room temperature at a rate of 2 °C/ 20 min. Single crystals suitable for X-ray diffraction were obtained in the form of black bars in ca 20% yield.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The asymmetric unit of the title compound.
	Fig. 2. The 1-D zigzag chain structure of the title compoud.

Poly[µ₂-chlorido-dichlorido[µ₂-4'-(4-pyridyl)-2,2':6',2''- terpyridine]copper(I)copper(II)] top

Crystal data top

[Cu₂Cl₃(C₂₀H₁₄N₄)]	Z = 2
M_r = 543.78	F(000) = 542
Triclinic, P1	D_x = 1.849 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.1389 (8) Å	Cell parameters from 1056 reflections
b = 9.8161 (10) Å	θ = 2.4–26.0°
c = 12.4823 (13) Å	µ = 2.60 mm⁻¹
α = 79.512 (2)°	T = 294 K
β = 85.036 (2)°	Block, black
γ = 88.202 (2)°	0.15 × 0.12 × 0.10 mm
V = 976.78 (17) Å³

Data collection top

Bruker SMART diffractometer	3778 independent reflections
Radiation source: fine-focus sealed tube	3391 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.014
ϕ and ω scans	θ_max = 26.0°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→9
T_min = 0.694, T_max = 0.771	k = −12→12
7840 measured reflections	l = −15→15

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)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.072	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0383P)² + 0.3983P] where P = (F_o² + 2F_c²)/3
3778 reflections	(Δ/σ)_max = 0.002
262 parameters	Δρ_max = 0.40 e Å⁻³
0 restraints	Δρ_min = −0.34 e Å⁻³

Crystal data top

[Cu₂Cl₃(C₂₀H₁₄N₄)]	γ = 88.202 (2)°
M_r = 543.78	V = 976.78 (17) Å³
Triclinic, P1	Z = 2
a = 8.1389 (8) Å	Mo Kα radiation
b = 9.8161 (10) Å	µ = 2.60 mm⁻¹
c = 12.4823 (13) Å	T = 294 K
α = 79.512 (2)°	0.15 × 0.12 × 0.10 mm
β = 85.036 (2)°

Data collection top

Bruker SMART diffractometer	3778 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3391 reflections with I > 2σ(I)
T_min = 0.694, T_max = 0.771	R_int = 0.014
7840 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.027	0 restraints
wR(F²) = 0.072	H-atom parameters constrained
S = 1.06	Δρ_max = 0.40 e Å⁻³
3778 reflections	Δρ_min = −0.34 e Å⁻³
262 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
Cu1	1.55686 (3)	0.36696 (3)	−0.35707 (2)	0.02849 (9)
Cu2	1.49349 (3)	0.14312 (3)	−0.05428 (3)	0.04087 (10)
Cl1	1.36557 (7)	−0.05058 (6)	−0.10452 (5)	0.03600 (14)
Cl3	1.68201 (7)	0.25884 (6)	−0.18347 (5)	0.03968 (15)
Cl2	1.73952 (7)	0.30031 (7)	−0.48213 (5)	0.04485 (16)
C16	0.4539 (2)	0.3584 (2)	0.30399 (17)	0.0271 (4)
N2	0.6324 (2)	0.54582 (18)	0.28869 (14)	0.0266 (4)
N4	1.2937 (2)	0.24557 (19)	0.00438 (16)	0.0332 (4)
N3	0.3521 (2)	0.43980 (19)	0.35802 (14)	0.0299 (4)
N1	0.6210 (2)	0.77686 (18)	0.35354 (14)	0.0288 (4)
C11	1.3087 (3)	0.3651 (2)	0.03817 (19)	0.0333 (5)
H11	1.4103	0.4084	0.0239	0.040*
C15	0.6150 (2)	0.4212 (2)	0.26284 (17)	0.0265 (4)
C14	0.7417 (2)	0.3610 (2)	0.20518 (17)	0.0282 (4)
H14	0.7274	0.2755	0.1854	0.034*
C9	1.0297 (2)	0.3681 (2)	0.11560 (17)	0.0273 (4)
C8	0.8918 (2)	0.4302 (2)	0.17696 (17)	0.0260 (4)
C6	0.7742 (2)	0.6135 (2)	0.26509 (17)	0.0270 (4)
C7	0.9077 (2)	0.5576 (2)	0.20962 (17)	0.0286 (4)
H7	1.0068	0.6047	0.1944	0.034*
C10	1.1832 (3)	0.4291 (2)	0.09312 (19)	0.0324 (5)
H10	1.2014	0.5126	0.1150	0.039*
C1	0.6025 (3)	0.8956 (2)	0.39099 (19)	0.0355 (5)
H1	0.5002	0.9170	0.4237	0.043*
C3	0.8787 (3)	0.9570 (3)	0.3336 (2)	0.0464 (6)
H3	0.9655	1.0182	0.3272	0.056*
C18	0.2576 (3)	0.1787 (3)	0.3369 (2)	0.0415 (6)
H18	0.2260	0.0904	0.3308	0.050*
C4	0.9006 (3)	0.8347 (2)	0.2933 (2)	0.0404 (6)
H4	1.0018	0.8122	0.2598	0.049*
C5	0.7688 (3)	0.7472 (2)	0.30392 (17)	0.0286 (4)
C17	0.4102 (3)	0.2284 (2)	0.29147 (19)	0.0335 (5)
H17	0.4816	0.1749	0.2532	0.040*
C2	0.7283 (3)	0.9875 (3)	0.3832 (2)	0.0411 (6)
H2	0.7120	1.0691	0.4109	0.049*
C13	1.0125 (3)	0.2455 (3)	0.0776 (2)	0.0465 (7)
H13	0.9113	0.2014	0.0886	0.056*
C20	0.2040 (3)	0.3911 (3)	0.40001 (19)	0.0368 (5)
H20	0.1330	0.4468	0.4364	0.044*
C19	0.1529 (3)	0.2610 (3)	0.3913 (2)	0.0420 (6)
H19	0.0496	0.2296	0.4216	0.050*
C12	1.1452 (3)	0.1887 (3)	0.0232 (2)	0.0480 (7)
H12	1.1300	0.1065	−0.0014	0.058*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.02035 (14)	0.03193 (16)	0.03487 (16)	0.00211 (10)	0.00583 (10)	−0.01466 (11)
Cu2	0.02869 (16)	0.04265 (18)	0.0509 (2)	0.00035 (12)	0.01106 (13)	−0.01440 (14)
Cl1	0.0362 (3)	0.0355 (3)	0.0399 (3)	−0.0021 (2)	−0.0025 (2)	−0.0165 (2)
Cl3	0.0261 (3)	0.0494 (3)	0.0401 (3)	−0.0083 (2)	0.0011 (2)	0.0003 (3)
Cl2	0.0350 (3)	0.0568 (4)	0.0461 (3)	0.0020 (3)	0.0134 (2)	−0.0265 (3)
C16	0.0199 (10)	0.0300 (11)	0.0308 (11)	0.0016 (8)	0.0031 (8)	−0.0069 (9)
N2	0.0191 (8)	0.0270 (9)	0.0340 (9)	0.0018 (7)	0.0035 (7)	−0.0092 (7)
N4	0.0229 (9)	0.0345 (10)	0.0428 (11)	0.0016 (7)	0.0081 (8)	−0.0140 (8)
N3	0.0234 (9)	0.0323 (10)	0.0334 (10)	0.0012 (7)	0.0061 (7)	−0.0085 (8)
N1	0.0244 (9)	0.0311 (9)	0.0335 (9)	0.0033 (7)	−0.0003 (7)	−0.0143 (8)
C11	0.0208 (10)	0.0339 (12)	0.0455 (13)	−0.0020 (9)	0.0067 (9)	−0.0120 (10)
C15	0.0211 (10)	0.0263 (10)	0.0319 (11)	0.0001 (8)	0.0028 (8)	−0.0073 (8)
C14	0.0228 (10)	0.0270 (10)	0.0359 (11)	−0.0002 (8)	0.0051 (8)	−0.0121 (9)
C9	0.0217 (10)	0.0289 (11)	0.0315 (11)	0.0030 (8)	0.0033 (8)	−0.0092 (9)
C8	0.0211 (10)	0.0285 (11)	0.0291 (10)	0.0023 (8)	0.0016 (8)	−0.0094 (8)
C6	0.0203 (10)	0.0284 (11)	0.0331 (11)	0.0024 (8)	0.0015 (8)	−0.0099 (9)
C7	0.0199 (10)	0.0309 (11)	0.0365 (12)	−0.0011 (8)	0.0035 (8)	−0.0125 (9)
C10	0.0235 (11)	0.0306 (11)	0.0452 (13)	−0.0013 (9)	0.0034 (9)	−0.0149 (10)
C1	0.0316 (12)	0.0363 (12)	0.0416 (13)	0.0062 (10)	0.0012 (10)	−0.0184 (10)
C3	0.0365 (13)	0.0401 (14)	0.0682 (18)	−0.0090 (11)	−0.0012 (12)	−0.0244 (13)
C18	0.0294 (12)	0.0366 (13)	0.0583 (16)	−0.0068 (10)	0.0024 (11)	−0.0096 (11)
C4	0.0261 (11)	0.0393 (13)	0.0595 (15)	−0.0017 (10)	0.0031 (10)	−0.0213 (12)
C5	0.0238 (10)	0.0294 (11)	0.0342 (11)	0.0038 (8)	−0.0005 (8)	−0.0117 (9)
C17	0.0232 (11)	0.0334 (12)	0.0444 (13)	−0.0002 (9)	0.0043 (9)	−0.0115 (10)
C2	0.0433 (14)	0.0348 (13)	0.0504 (14)	0.0015 (10)	−0.0019 (11)	−0.0231 (11)
C13	0.0246 (11)	0.0452 (14)	0.0749 (18)	−0.0108 (10)	0.0186 (11)	−0.0334 (13)
C20	0.0240 (11)	0.0434 (13)	0.0411 (13)	0.0019 (10)	0.0092 (9)	−0.0087 (10)
C19	0.0225 (11)	0.0462 (14)	0.0538 (15)	−0.0075 (10)	0.0082 (10)	−0.0044 (12)
C12	0.0326 (13)	0.0413 (14)	0.0762 (19)	−0.0075 (11)	0.0179 (12)	−0.0361 (13)

Geometric parameters (Å, º) top

Cu1—N2ⁱ	1.9466 (16)	C14—H14	0.9300
Cu1—N1ⁱ	2.0455 (18)	C9—C10	1.387 (3)
Cu1—N3ⁱ	2.0557 (18)	C9—C13	1.387 (3)
Cu1—Cl2	2.2325 (6)	C9—C8	1.483 (3)
Cu1—Cl3	2.5172 (6)	C8—C7	1.397 (3)
Cu2—N4	2.0374 (18)	C6—C7	1.390 (3)
Cu2—Cl3	2.2933 (6)	C6—C5	1.478 (3)
Cu2—Cl1ⁱⁱ	2.3964 (7)	C7—H7	0.9300
Cu2—Cl1	2.4007 (6)	C10—H10	0.9300
Cu2—Cu2ⁱⁱ	2.8917 (7)	C1—C2	1.371 (3)
Cl1—Cu2ⁱⁱ	2.3964 (7)	C1—H1	0.9300
C16—N3	1.355 (3)	C3—C2	1.373 (3)
C16—C17	1.375 (3)	C3—C4	1.385 (3)
C16—C15	1.477 (3)	C3—H3	0.9300
N2—C6	1.333 (3)	C18—C19	1.377 (3)
N2—C15	1.335 (3)	C18—C17	1.385 (3)
N2—Cu1ⁱ	1.9466 (16)	C18—H18	0.9300
N4—C11	1.330 (3)	C4—C5	1.377 (3)
N4—C12	1.332 (3)	C4—H4	0.9300
N3—C20	1.339 (3)	C17—H17	0.9300
N3—Cu1ⁱ	2.0557 (18)	C2—H2	0.9300
N1—C1	1.332 (3)	C13—C12	1.382 (3)
N1—C5	1.353 (3)	C13—H13	0.9300
N1—Cu1ⁱ	2.0455 (18)	C20—C19	1.381 (3)
C11—C10	1.380 (3)	C20—H20	0.9300
C11—H11	0.9300	C19—H19	0.9300
C15—C14	1.385 (3)	C12—H12	0.9300
C14—C8	1.403 (3)

N2ⁱ—Cu1—N1ⁱ	78.97 (7)	C10—C9—C8	121.92 (19)
N2ⁱ—Cu1—N3ⁱ	79.19 (7)	C13—C9—C8	121.8 (2)
N1ⁱ—Cu1—N3ⁱ	156.19 (7)	C7—C8—C14	118.17 (18)
N2ⁱ—Cu1—Cl2	162.20 (6)	C7—C8—C9	121.33 (19)
N1ⁱ—Cu1—Cl2	99.27 (5)	C14—C8—C9	120.49 (19)
N3ⁱ—Cu1—Cl2	98.61 (5)	N2—C6—C7	120.70 (19)
N2ⁱ—Cu1—Cl3	96.91 (5)	N2—C6—C5	112.78 (17)
N1ⁱ—Cu1—Cl3	97.93 (5)	C7—C6—C5	126.51 (19)
N3ⁱ—Cu1—Cl3	93.99 (5)	C6—C7—C8	119.42 (19)
Cl2—Cu1—Cl3	100.87 (2)	C6—C7—H7	120.3
N4—Cu2—Cl3	120.37 (6)	C8—C7—H7	120.3
N4—Cu2—Cl1ⁱⁱ	104.34 (6)	C11—C10—C9	119.6 (2)
Cl3—Cu2—Cl1ⁱⁱ	107.93 (2)	C11—C10—H10	120.2
N4—Cu2—Cl1	101.32 (6)	C9—C10—H10	120.2
Cl3—Cu2—Cl1	115.66 (2)	N1—C1—C2	122.6 (2)
Cl1ⁱⁱ—Cu2—Cl1	105.86 (2)	N1—C1—H1	118.7
N4—Cu2—Cu2ⁱⁱ	111.61 (6)	C2—C1—H1	118.7
Cl3—Cu2—Cu2ⁱⁱ	127.92 (2)	C2—C3—C4	119.6 (2)
Cl1ⁱⁱ—Cu2—Cu2ⁱⁱ	52.998 (16)	C2—C3—H3	120.2
Cl1—Cu2—Cu2ⁱⁱ	52.861 (18)	C4—C3—H3	120.2
Cu2ⁱⁱ—Cl1—Cu2	74.14 (2)	C19—C18—C17	119.5 (2)
Cu2—Cl3—Cu1	112.90 (2)	C19—C18—H18	120.2
N3—C16—C17	122.26 (19)	C17—C18—H18	120.2
N3—C16—C15	113.85 (18)	C5—C4—C3	118.4 (2)
C17—C16—C15	123.88 (18)	C5—C4—H4	120.8
C6—N2—C15	121.47 (17)	C3—C4—H4	120.8
C6—N2—Cu1ⁱ	119.54 (14)	N1—C5—C4	121.9 (2)
C15—N2—Cu1ⁱ	118.95 (14)	N1—C5—C6	113.76 (18)
C11—N4—C12	116.29 (19)	C4—C5—C6	124.37 (19)
C11—N4—Cu2	121.51 (15)	C16—C17—C18	118.6 (2)
C12—N4—Cu2	121.71 (15)	C16—C17—H17	120.7
C20—N3—C16	118.36 (19)	C18—C17—H17	120.7
C20—N3—Cu1ⁱ	127.42 (15)	C1—C2—C3	118.8 (2)
C16—N3—Cu1ⁱ	114.11 (14)	C1—C2—H2	120.6
C1—N1—C5	118.65 (19)	C3—C2—H2	120.6
C1—N1—Cu1ⁱ	126.56 (15)	C12—C13—C9	120.2 (2)
C5—N1—Cu1ⁱ	114.75 (14)	C12—C13—H13	119.9
N4—C11—C10	124.2 (2)	C9—C13—H13	119.9
N4—C11—H11	117.9	N3—C20—C19	122.4 (2)
C10—C11—H11	117.9	N3—C20—H20	118.8
N2—C15—C14	120.84 (19)	C19—C20—H20	118.8
N2—C15—C16	113.24 (17)	C18—C19—C20	118.9 (2)
C14—C15—C16	125.90 (19)	C18—C19—H19	120.6
C15—C14—C8	119.30 (19)	C20—C19—H19	120.6
C15—C14—H14	120.4	N4—C12—C13	123.4 (2)
C8—C14—H14	120.4	N4—C12—H12	118.3
C10—C9—C13	116.26 (19)	C13—C12—H12	118.3

Symmetry codes: (i) −x+2, −y+1, −z; (ii) −x+3, −y, −z.

Experimental details

Crystal data
Chemical formula	[Cu₂Cl₃(C₂₀H₁₄N₄)]
M_r	543.78
Crystal system, space group	Triclinic, P1
Temperature (K)	294
a, b, c (Å)	8.1389 (8), 9.8161 (10), 12.4823 (13)
α, β, γ (°)	79.512 (2), 85.036 (2), 88.202 (2)
V (Å³)	976.78 (17)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.60
Crystal size (mm)	0.15 × 0.12 × 0.10

Data collection
Diffractometer	Bruker SMART diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.694, 0.771
No. of measured, independent and observed [I > 2σ(I)] reflections	7840, 3778, 3391
R_int	0.014
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.027, 0.072, 1.06
No. of reflections	3778
No. of parameters	262
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.40, −0.34

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

References

Bruker (1998). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Hou, L., Li, D., Shi, W.-J., Yin, Y.-G. & Ng, S. W. (2005). Inorg. Chem. 44, 7825–7832. Web of Science CSD CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (1996). University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zhang, S.-S., Zhan, S.-Z., Li, M., Peng, R. & Li, D. (2007). Inorg. Chem. 46, 4365–4367. Web of Science CSD CrossRef PubMed CAS Google Scholar

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