Bis[iodidobis(1,10-phenanthroline-κ2N,N′)copper(II)] tetra­iodidocadmate(II)

Cao, M.-L.; Fang, X.; Zhang, Y.-J.; Yu, H.-Y.; Wang, J.-D.

doi:10.1107/S1600536807025329

Bis[iodidobis(1,10-phenanthroline-κ²N,N′)copper(II)] tetraiodidocadmate(II)

M.-L. Cao, X. Fang, Y.-J. Zhang, H.-Y. Yu and J.-D. Wang

A new mixed-metal complex, [CuI(C₁₂H₈N₂)₂]₂[CdI₄], with an asymmetric unit consisting of one [CuI(phen)₂]⁺ cation (phen = 1,10-phenanthroline) and half of a [CdI₄]²⁻ anion lying on a twofold rotation axis, has been synthesized. The Cu²⁺ ion in the [CuI(phen)₂]⁺ cation is five-coordinated by two bidentate phenanthroline ligands and an iodide ligand. The crystal packing is stabilized by intermolecular C—H

I hydrogen bonds.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807025329/im2017sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807025329/im2017Isup2.hkl Contains datablock I

CCDC reference: 654686

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Key indicators

Single-crystal X-ray study
T = 173 K
Mean (Wave) = 0.000 Å
R factor = 0.033
wR factor = 0.085
Data-to-parameter ratio = 19.7

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No syntax errors found



Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      1.059
            Tmax scaled      0.170 Tmin scaled      0.106

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   0 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

Considerable attention has been paid to heteronuclear metal complexes. At present, a variety of mixed metal complexes have been reported. (Chesnut et al., 1999. Ferbinteanu et al., 1998. Shiren et al., 2002.). Here, a new mixed metal complex is obtained under low temperature conditions. The asymmetric unit of the title compound, (I), contains one [CuI(phen)₂]⁺ cation and a CdI₂ subunit of the CdI₄ dianion with the cadmium atom observed on a crystallographic twofold axis. In the cation, four N atoms of two bidentate phenanthroline ligands and one iodo ligand form an approximately trigonal-bipyramidal arrangement around the Cu²⁺ ion, with atoms I3, N1 and N4 occupying equatorial positions whereas N2 and N3 occupy the axial positions (Fig. 1). The equatorial plane (Table 1) is distorted with angles of 124.07 (9)° (N1—Cu1—I3), 125.98 (9)° (N4—Cu1—I3), and 109.94 (13)° (N1—Cu1—N4). In the crystal structure of (I), the crystal packing is stabilized by intermolecular I—H interactions between I atoms of the anion and H atoms of the phenanthroline ligands with distances of 3.15 Å, as listed in Table 1. In addition, one of the iodine atoms of the anion (I1) is positioned over the adjacent ring of one of the phenanthroline ligands (C13—C17—C24) with a distance of 3.535 Å.

Related literature top

For related literature see: Chesnut et al. (1999); Ferbinteanu et al. (1998); Shiren et al. (2002); Bowmaker et al. (1973); Boys (1988); Boys et al. (1981); Healy et al. (1985); Pallenberg et al. (1995); Yang et al. (2004).

Experimental top

The title compound was prepared at room temperature. Firstly, CdI₂ (0.0366 g, 0.1 mmol) and phen (0.018 g, 0.1 mmol) were slowly added to 5 ml DMF and stirred for 30 min. Meanwhile, CuI (0.0191 g, 0.1 mmol) was added to another 5 ml of DMF, followed by slow addition of KI (0.0116 g,0.1 mmol) in 10 ml DMF until the solution became clear, and stirred for 30 min. Then the two solutions were mixed, stirred for 20 min, and filtered. After the solvent was slowly evaporated at -5°C, dark-purple crystals of the title compound weres obtained.

Structure description top

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Figures top

Fig. 1. The molecular structure of (I), with atom labels and 50% probability displacement ellipsoids for non-H atoms.

Bis[iodidobis(1,10-phenanthroline-κ²N,N')copper(II)] tetraiodidocadmate(II) top

Crystal data top

[CuI(C₁₂H₈N₂)₂]₂[CdI₄]	F(000) = 3200
M_r = 1721.70	D_x = 2.250 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C2yc	Cell parameters from 24621 reflections
a = 21.0726 (5) Å	θ = 6.1–55.0°
b = 15.4727 (5) Å	µ = 4.93 mm⁻¹
c = 15.5907 (4) Å	T = 173 K
β = 90.991 (1)°	Block, black
V = 5082.6 (2) Å³	0.66 × 0.41 × 0.36 mm
Z = 4

Data collection top

Rigaku R-AXIS SPIDER diffractometer	5821 independent reflections
Radiation source: fine-focus sealed tube	5537 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.061
Detector resolution: 10 pixels mm^-1	θ_max = 27.5°, θ_min = 3.1°
ω oscillation scans	h = −27→27
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −20→18
T_min = 0.10, T_max = 0.16	l = −20→20
24621 measured reflections

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	Only H-atom displacement parameters refined
wR(F²) = 0.085	w = 1/[σ²(F_o²) + (0.0235P)² + 27.9995P] where P = (F_o² + 2F_c²)/3
S = 1.11	(Δ/σ)_max = 0.002
5821 reflections	Δρ_max = 2.18 e Å⁻³
295 parameters	Δρ_min = −1.31 e Å⁻³
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00044 (4)

Crystal data top

[CuI(C₁₂H₈N₂)₂]₂[CdI₄]	V = 5082.6 (2) Å³
M_r = 1721.70	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 21.0726 (5) Å	µ = 4.93 mm⁻¹
b = 15.4727 (5) Å	T = 173 K
c = 15.5907 (4) Å	0.66 × 0.41 × 0.36 mm
β = 90.991 (1)°

Data collection top

Rigaku R-AXIS SPIDER diffractometer	5821 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	5537 reflections with I > 2σ(I)
T_min = 0.10, T_max = 0.16	R_int = 0.061
24621 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.033	0 restraints
wR(F²) = 0.085	Only H-atom displacement parameters refined
S = 1.11	w = 1/[σ²(F_o²) + (0.0235P)² + 27.9995P] where P = (F_o² + 2F_c²)/3
5821 reflections	Δρ_max = 2.18 e Å⁻³
295 parameters	Δρ_min = −1.31 e Å⁻³

Special details top

Experimental. collimator diameter: 0.800000 mm

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
I1	0.423976 (12)	0.574827 (17)	0.144226 (16)	0.02418 (9)
I2	0.564820 (16)	0.78122 (2)	0.13363 (3)	0.05017 (13)
I3	0.851339 (13)	0.54118 (2)	0.092126 (18)	0.03378 (10)
Cd1	0.5000	0.67667 (3)	0.2500	0.03004 (12)
Cu1	0.78535 (2)	0.55003 (3)	0.23361 (3)	0.02163 (12)
N3	0.70292 (15)	0.5289 (2)	0.1721 (2)	0.0233 (7)
N4	0.75284 (15)	0.4442 (2)	0.3055 (2)	0.0214 (6)
N2	0.86250 (15)	0.5681 (2)	0.3079 (2)	0.0239 (7)
N1	0.75895 (15)	0.6662 (2)	0.2927 (2)	0.0215 (6)
C1	0.70786 (18)	0.7152 (3)	0.2834 (3)	0.0240 (8)
H1	0.6774	0.6994	0.2425	0.029*
C2	0.69748 (19)	0.7896 (3)	0.3321 (3)	0.0261 (8)
H2	0.6609	0.8224	0.3233	0.031*
C3	0.7417 (2)	0.8138 (3)	0.3929 (3)	0.0264 (8)
H3	0.7354	0.8632	0.4257	0.032*
C4	0.79673 (19)	0.7635 (3)	0.4054 (2)	0.0242 (8)
C5	0.8465 (2)	0.7822 (3)	0.4664 (3)	0.0278 (8)
H5	0.8425	0.8302	0.5018	0.033*
C6	0.8982 (2)	0.7332 (3)	0.4742 (3)	0.0307 (9)
H6	0.9294	0.7476	0.5147	0.037*
C7	0.90659 (19)	0.6585 (3)	0.4211 (3)	0.0263 (8)
C8	0.9604 (2)	0.6047 (3)	0.4244 (3)	0.0334 (10)
H8	0.9934	0.6163	0.4629	0.040*
C9	0.9637 (2)	0.5352 (3)	0.3707 (3)	0.0353 (10)
H9	0.9990	0.4991	0.3728	0.042*
C10	0.9137 (2)	0.5183 (3)	0.3123 (3)	0.0315 (9)
H10	0.9166	0.4710	0.2758	0.038*
C11	0.80319 (18)	0.6898 (3)	0.3528 (2)	0.0211 (7)
C12	0.85850 (17)	0.6375 (3)	0.3612 (2)	0.0221 (7)
C13	0.6792 (2)	0.5724 (3)	0.1061 (3)	0.0315 (9)
H13	0.7019	0.6191	0.0851	0.038*
C14	0.6213 (2)	0.5511 (3)	0.0665 (3)	0.0359 (10)
H14	0.6060	0.5833	0.0203	0.043*
C15	0.5874 (2)	0.4826 (3)	0.0962 (3)	0.0340 (10)
H15	0.5491	0.4673	0.0699	0.041*
C16	0.61076 (18)	0.4357 (3)	0.1666 (3)	0.0270 (8)
C17	0.57891 (19)	0.3634 (3)	0.2041 (3)	0.0317 (9)
H17	0.5400	0.3457	0.1812	0.038*
C18	0.6040 (2)	0.3205 (3)	0.2716 (3)	0.0347 (10)
H18	0.5820	0.2737	0.2940	0.042*
C19	0.66377 (19)	0.3450 (3)	0.3098 (3)	0.0272 (8)
C20	0.6931 (2)	0.3022 (3)	0.3785 (3)	0.0344 (10)
H20	0.6738	0.2543	0.4029	0.041*
C21	0.7504 (2)	0.3312 (3)	0.4097 (3)	0.0329 (9)
H21	0.7703	0.3033	0.4556	0.039*
C22	0.7788 (2)	0.4031 (3)	0.3716 (3)	0.0259 (8)
H22	0.8174	0.4227	0.3937	0.031*
C23	0.66964 (18)	0.4619 (3)	0.2029 (2)	0.0223 (8)
C24	0.69596 (18)	0.4160 (3)	0.2747 (2)	0.0215 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
I1	0.02396 (14)	0.02735 (15)	0.02109 (14)	−0.00515 (9)	−0.00331 (9)	0.00105 (10)
I2	0.04088 (19)	0.03983 (18)	0.0688 (3)	−0.01745 (14)	−0.02675 (17)	0.02747 (17)
I3	0.02672 (15)	0.04954 (19)	0.02509 (15)	0.00118 (11)	0.00064 (11)	0.00351 (12)
Cd1	0.0284 (2)	0.0233 (2)	0.0379 (2)	0.000	−0.01419 (18)	0.000
Cu1	0.0176 (2)	0.0273 (2)	0.0198 (2)	−0.00080 (17)	−0.00559 (17)	0.00044 (19)
N3	0.0210 (15)	0.0285 (17)	0.0203 (15)	0.0005 (13)	−0.0034 (12)	−0.0005 (14)
N4	0.0221 (15)	0.0256 (16)	0.0166 (14)	0.0007 (12)	−0.0001 (12)	−0.0032 (13)
N2	0.0191 (15)	0.0297 (17)	0.0227 (16)	−0.0014 (13)	−0.0051 (12)	0.0016 (14)
N1	0.0179 (15)	0.0276 (16)	0.0189 (15)	−0.0030 (12)	−0.0015 (12)	0.0052 (13)
C1	0.0188 (17)	0.029 (2)	0.0241 (18)	−0.0022 (14)	−0.0010 (14)	0.0052 (16)
C2	0.0236 (19)	0.029 (2)	0.026 (2)	0.0024 (15)	0.0033 (15)	0.0067 (17)
C3	0.033 (2)	0.0242 (19)	0.0220 (19)	−0.0041 (16)	0.0059 (16)	0.0006 (16)
C4	0.0267 (19)	0.0288 (19)	0.0170 (17)	−0.0076 (15)	0.0010 (14)	0.0035 (16)
C5	0.034 (2)	0.033 (2)	0.0168 (17)	−0.0085 (17)	−0.0023 (15)	−0.0005 (16)
C6	0.030 (2)	0.041 (2)	0.0210 (19)	−0.0128 (18)	−0.0066 (16)	0.0003 (18)
C7	0.0230 (19)	0.035 (2)	0.0206 (18)	−0.0070 (16)	−0.0058 (15)	0.0044 (17)
C8	0.023 (2)	0.047 (3)	0.030 (2)	−0.0036 (18)	−0.0103 (16)	0.004 (2)
C9	0.022 (2)	0.048 (3)	0.036 (2)	0.0061 (18)	−0.0071 (17)	0.005 (2)
C10	0.025 (2)	0.037 (2)	0.032 (2)	0.0023 (17)	−0.0036 (17)	−0.0007 (19)
C11	0.0214 (18)	0.0264 (18)	0.0156 (16)	−0.0062 (14)	−0.0002 (13)	0.0029 (15)
C12	0.0202 (17)	0.0293 (19)	0.0167 (16)	−0.0047 (14)	−0.0030 (14)	0.0044 (15)
C13	0.032 (2)	0.037 (2)	0.025 (2)	−0.0009 (17)	−0.0080 (17)	0.0003 (18)
C14	0.029 (2)	0.047 (3)	0.031 (2)	0.0085 (19)	−0.0121 (18)	0.000 (2)
C15	0.023 (2)	0.047 (3)	0.032 (2)	0.0059 (18)	−0.0073 (17)	−0.013 (2)
C16	0.0177 (18)	0.036 (2)	0.027 (2)	0.0021 (15)	0.0010 (15)	−0.0142 (18)
C17	0.0190 (18)	0.041 (2)	0.035 (2)	−0.0043 (17)	0.0045 (16)	−0.014 (2)
C18	0.029 (2)	0.039 (2)	0.036 (2)	−0.0108 (18)	0.0109 (18)	−0.012 (2)
C19	0.0259 (19)	0.030 (2)	0.026 (2)	−0.0023 (16)	0.0066 (15)	−0.0067 (17)
C20	0.042 (3)	0.030 (2)	0.032 (2)	−0.0050 (18)	0.0096 (19)	−0.0002 (19)
C21	0.043 (3)	0.033 (2)	0.022 (2)	0.0033 (19)	−0.0035 (17)	0.0037 (18)
C22	0.028 (2)	0.030 (2)	0.0200 (18)	0.0020 (16)	−0.0019 (15)	−0.0018 (16)
C23	0.0176 (17)	0.032 (2)	0.0179 (17)	0.0024 (14)	0.0024 (13)	−0.0083 (15)
C24	0.0204 (17)	0.0261 (18)	0.0181 (17)	0.0019 (14)	0.0039 (14)	−0.0068 (15)

Geometric parameters (Å, º) top

I1—Cd1	2.7709 (3)	C7—C12	1.404 (5)
I2—Cd1	2.8036 (4)	C7—C8	1.407 (6)
I3—Cu1	2.6314 (6)	C8—C9	1.365 (7)
Cd1—I1ⁱ	2.7708 (3)	C8—H8	0.9300
Cd1—I2ⁱ	2.8036 (4)	C9—C10	1.405 (6)
Cu1—N3	1.996 (3)	C9—H9	0.9300
Cu1—N2	1.999 (3)	C10—H10	0.9300
Cu1—N1	2.099 (3)	C11—C12	1.424 (5)
Cu1—N4	2.105 (3)	C13—C14	1.397 (6)
N3—C13	1.321 (5)	C13—H13	0.9300
N3—C23	1.346 (5)	C14—C15	1.362 (7)
N4—C22	1.321 (5)	C14—H14	0.9300
N4—C24	1.356 (5)	C15—C16	1.397 (6)
N2—C10	1.327 (5)	C15—H15	0.9300
N2—C12	1.362 (5)	C16—C23	1.414 (5)
N1—C1	1.323 (5)	C16—C17	1.435 (6)
N1—C11	1.360 (5)	C17—C18	1.344 (7)
C1—C2	1.399 (6)	C17—H17	0.9300
C1—H1	0.9300	C18—C19	1.436 (6)
C2—C3	1.370 (6)	C18—H18	0.9300
C2—H2	0.9300	C19—C20	1.394 (7)
C3—C4	1.407 (6)	C19—C24	1.407 (6)
C3—H3	0.9300	C20—C21	1.370 (7)
C4—C11	1.413 (6)	C20—H20	0.9300
C4—C5	1.433 (5)	C21—C22	1.401 (6)
C5—C6	1.331 (6)	C21—H21	0.9300
C5—H5	0.9300	C22—H22	0.9300
C6—C7	1.434 (6)	C23—C24	1.429 (6)
C6—H6	0.9300

I1—Cd1—I1ⁱ	110.681 (18)	C9—C8—H8	120.2
I1—Cd1—I2ⁱ	115.477 (9)	C7—C8—H8	120.2
I1ⁱ—Cd1—I2ⁱ	103.070 (9)	C8—C9—C10	119.8 (4)
I1—Cd1—I2	103.070 (9)	C8—C9—H9	120.1
I1ⁱ—Cd1—I2	115.477 (9)	C10—C9—H9	120.1
I2ⁱ—Cd1—I2	109.52 (2)	N2—C10—C9	121.8 (4)
N3—Cu1—N2	173.27 (14)	N2—C10—H10	119.1
N3—Cu1—N1	96.64 (13)	C9—C10—H10	119.1
N2—Cu1—N1	81.10 (13)	N1—C11—C4	123.0 (4)
N3—Cu1—N4	80.80 (13)	N1—C11—C12	117.5 (3)
N2—Cu1—N4	93.96 (13)	C4—C11—C12	119.5 (3)
N1—Cu1—N4	109.94 (13)	N2—C12—C7	122.5 (4)
N3—Cu1—I3	93.26 (10)	N2—C12—C11	116.8 (3)
N2—Cu1—I3	93.24 (10)	C7—C12—C11	120.6 (4)
N1—Cu1—I3	124.07 (9)	N3—C13—C14	122.7 (4)
N4—Cu1—I3	125.98 (9)	N3—C13—H13	118.7
C13—N3—C23	118.5 (4)	C14—C13—H13	118.7
C13—N3—Cu1	127.3 (3)	C15—C14—C13	119.4 (4)
C23—N3—Cu1	114.2 (3)	C15—C14—H14	120.3
C22—N4—C24	118.2 (4)	C13—C14—H14	120.3
C22—N4—Cu1	131.0 (3)	C14—C15—C16	119.4 (4)
C24—N4—Cu1	110.8 (3)	C14—C15—H15	120.3
C10—N2—C12	119.0 (3)	C16—C15—H15	120.3
C10—N2—Cu1	127.0 (3)	C15—C16—C23	117.4 (4)
C12—N2—Cu1	113.9 (3)	C15—C16—C17	124.4 (4)
C1—N1—C11	117.9 (4)	C23—C16—C17	118.2 (4)
C1—N1—Cu1	131.6 (3)	C18—C17—C16	121.6 (4)
C11—N1—Cu1	110.4 (3)	C18—C17—H17	119.2
N1—C1—C2	123.2 (4)	C16—C17—H17	119.2
N1—C1—H1	118.4	C17—C18—C19	121.6 (4)
C2—C1—H1	118.4	C17—C18—H18	119.2
C3—C2—C1	119.3 (4)	C19—C18—H18	119.2
C3—C2—H2	120.3	C20—C19—C24	117.4 (4)
C1—C2—H2	120.3	C20—C19—C18	124.6 (4)
C2—C3—C4	119.6 (4)	C24—C19—C18	118.0 (4)
C2—C3—H3	120.2	C21—C20—C19	119.6 (4)
C4—C3—H3	120.2	C21—C20—H20	120.2
C3—C4—C11	116.9 (3)	C19—C20—H20	120.2
C3—C4—C5	125.0 (4)	C20—C21—C22	119.4 (4)
C11—C4—C5	118.1 (4)	C20—C21—H21	120.3
C6—C5—C4	122.3 (4)	C22—C21—H21	120.3
C6—C5—H5	118.8	N4—C22—C21	122.6 (4)
C4—C5—H5	118.8	N4—C22—H22	118.7
C5—C6—C7	121.0 (4)	C21—C22—H22	118.7
C5—C6—H6	119.5	N3—C23—C16	122.5 (4)
C7—C6—H6	119.5	N3—C23—C24	117.7 (3)
C12—C7—C8	117.3 (4)	C16—C23—C24	119.8 (4)
C12—C7—C6	118.4 (4)	N4—C24—C19	122.9 (4)
C8—C7—C6	124.3 (4)	N4—C24—C23	116.5 (4)
C9—C8—C7	119.7 (4)	C19—C24—C23	120.6 (4)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···I2	0.93	3.16	3.916 (4)	140
C5—H5···I1ⁱⁱ	0.93	3.15	3.884 (4)	138

Symmetry code: (ii) x+1/2, −y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formula	[CuI(C₁₂H₈N₂)₂]₂[CdI₄]
M_r	1721.70
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	173
a, b, c (Å)	21.0726 (5), 15.4727 (5), 15.5907 (4)
β (°)	90.991 (1)
V (Å³)	5082.6 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	4.93
Crystal size (mm)	0.66 × 0.41 × 0.36

Data collection
Diffractometer	Rigaku R-AXIS SPIDER
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.10, 0.16
No. of measured, independent and observed [I > 2σ(I)] reflections	24621, 5821, 5537
R_int	0.061
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.033, 0.085, 1.11
No. of reflections	5821
No. of parameters	295
H-atom treatment	Only H-atom displacement parameters refined
	w = 1/[σ²(F_o²) + (0.0235P)² + 27.9995P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	2.18, −1.31

Computer programs: RAPID-AUTO (Rigaku, 2004), RAPID-AUTO, SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b), SHELXTL.