Bis(tetra­propyl­ammonium) di-μ3-iodido-di-μ2-iodido-diiodidodi­pyridine­tetra­copper(I)

Jalilian, E.

doi:10.1107/S1600536810010202

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 4| April 2010| Page m431

doi:10.1107/S1600536810010202

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Bis(tetrapropylammonium) di-μ₃-iodido-di-μ₂-iodido-diiodidodipyridinetetracopper(I)

Ehsan Jalilian ^a ^*

^aDepartment of Environmental and Material Chemistry, Arrhenius Laboratory, Stockholm University, 106 91 Stockholm, Sweden
^*Correspondence e-mail: ehsan.jalilian@mmk.su.se

(Received 15 March 2010; accepted 18 March 2010; online 24 March 2010)

The title compound, (C₁₂H₂₈N)₂[Cu_3.194I₆(C₅H₅N)₂] was prepared from reaction of copper powder, copper(I) oxide, hydroiodic acid, tetrapropylammonium iodide and pyridine under hydrothermal conditions. In the centrosymmetric Cu₄I₆²⁻ anion, one Cu site is in a trigonal-planar coordination while the second Cu site, which is only partially occupied [site occupancy of 0.5968 (16)], is surroundedby three iodine atoms and one pyridine molecule in a distorted tetrahedral coordination.

Related literature

For further structural motifs and the luminescence properties of copper(I)iodide with substituted pyridine, see Cariati et al. (2005 ). For the extinction correction, see: Becker & Coppens (1974 ).

Experimental

Crystal data

(C₁₂H₂₈N)₂[Cu_3.194I₆(C₅H₅N)₂]
M_r = 1495.3
Triclinic, $[P \overline 1]$
a = 8.8974 (2) Å
b = 11.8076 (3) Å
c = 12.2176 (2) Å
α = 73.2442 (18)°
β = 78.5398 (17)°
γ = 81.4137 (18)°
V = 1198.74 (5) Å³
Z = 1
Mo Kα radiation
μ = 5.29 mm⁻¹
T = 100 K
0.47 × 0.17 × 0.13 mm

Data collection

Oxford Diffraction Xcalibur3 diffractometer with a Sapphire-3 CCD detector
Absorption correction: Gaussian (CrysAlis RED; Oxford Diffraction, 2008 $[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]$ ) T_min = 0.209, T_max = 0.623
38326 measured reflections
7574 independent reflections
6526 reflections with I > 3σ(I)
R_int = 0.020

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.068
S = 1.02
7574 reflections
219 parameters
H-atom parameters constrained
Δρ_max = 1.05 e Å⁻³
Δρ_min = −0.53 e Å⁻³

Data collection: CrysAlis CCD (Oxford Diffraction, 2008 $[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2008 $[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SUPERFLIP (Oszlányi & Sütő, 2004 ); program(s) used to refine structure: JANA2000 (Petříček et al., 2000 ); molecular graphics: DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: JANA2000.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810010202/jh2137sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810010202/jh2137Isup2.hkl

checkCIF report

Comment top

Due to the wide variation in molecular structure, halocuprates(I) exhibit a very interesting structural chemistry. The most important factor to this structural diversity is the fact that Cu(I) can accept trigonal planar coordination, tetrahedral coordination as well as less defined intermediate arrangements. The further linkage of these units, triangles by corner-sharing or edge-sharing, tetrahedra also by face sharing yields further structural flexibility. Many different version of oligometric and polymeric species in Cu(I)X (X=Cl,Br, I) have been discovered in copper (I) halide based systems containing inflexible N- donor ligands. Stoichiometry and connectivity are dependent on the size and the coordination number of the cation that participate in the structure. The compound presented here 2[(C₁₂H₂₈N)⁺ [I₃ Cu_1.597 N C₅ H₅]^- ] (I), is prepared from reaction between copper powder, copperoxide, tetra n-propylammoniumiodide, pyridine and hydroiodic acid. The anion in (I) has a range of Cu–I distances [ 2.5200 (3)–2.7752 (6) Å] while the I–Cu–I angles spread over large range [108.039 (16)–122.009 (14)°]. One of the two independent Cu positions is clearly under-occupied (Cu2, occ ≈ 0.6). This non-stoichiometry leads to local relaxations that can be seen as anomalously large and anisotropic thermal parameters on the surrounding I neighbours. The compound is light yellow in color, and it is well known that Cu cannot attain the divalent oxidation state in direct contact with iodide, and therefore we conclude that all Cu is in the monovalent state. The charge balance must instead be maintained by the protonation of either the pyridine unit or the Cu_4-xI₆ -cluster unit, a likely scenario since the synthesis is run at a low pH value.

The attached pyridine unit is a typical pyridine with N–C and C–C ranges [ 1.345 (3)–1.349 (3) Å and 1.359 (5)–1.398 (4)Å respectively] The angle C–N–C is 119.2 (2)° while (N/)C–C–C the angles ranges [ 118.4 (2)–120.8 (2)°]. The cation is a regular tetra propylammonium ion with N–C and C–C distances range [1.518 (3)–1.521 (3) Å and 1.516 (3)–1.542 (3)Å respectively], and the C–N–C, (N/)C–C–C angels range between [107.99 (16)–111.36 (15)° and 108.40 (19)–115.60 (18)°].

Related literature top

For further structural motifs and the luminescence properties of copper(I)iodide with substituted pyridine, see Cariati et al. (2005). For the extinction correction, see: Becker & Coppens (1974).

Experimental top

Copper powder (2.854 mmol), copper(I)oxide (2.827 mmol), hydroiodic acid (7.6 mmol) tetra n-propylammonium iodide (3.101 mmol) and pyridine (12.958 mmol) were put into an autoclave and heated at 165 °C for 19 h. It resulted in yellow crystals that luminesce vividly under UV light.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2008); cell refinement: CrysAlis RED (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: SUPERFLIP (Oszlányi & Sütő, 2004); program(s) used to refine structure: JANA2000 (Petricek et al., 2000); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: JANA2000 (Petricek et al., 2000).

Figures top

Fig. 1. Molecular structure with atom labelling scheme for the I—Cu-Pyridine anion and the tetrapropeylammonium cation in (I). Non H atoms are shown as 50% probability displacement ellipsoids.

Bis(tetrapropylammonium) di-µ₃-iodido-di-µ₂-iodido-diiodidodipyridinetetracopper(I) top

Crystal data top

(C₁₂H₂₈N)₂[Cu_3.194I₆(C₅H₅N)₂]	Z = 1
M_r = 1495.3	F(000) = 708.8
Triclinic, P1	D_x = 2.071 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71069 Å
a = 8.8974 (2) Å	Cell parameters from 27591 reflections
b = 11.8076 (3) Å	θ = 4.3–32.2°
c = 12.2176 (2) Å	µ = 5.29 mm⁻¹
α = 73.2442 (18)°	T = 100 K
β = 78.5398 (17)°	Rodd, yellow
γ = 81.4137 (18)°	0.47 × 0.17 × 0.13 mm
V = 1198.74 (5) Å³

Data collection top

Oxford Diffraction Xcalibur3 diffractometer with a Sapphire-3 CCD detector	7574 independent reflections
Radiation source: Enhance (Mo) X-ray source	6526 reflections with I > 3σ(I)
Graphite monochromator	R_int = 0.020
Detector resolution: 16.5467 pixels mm^-1	θ_max = 32.2°, θ_min = 4.3°
ω scans	h = −13→13
Absorption correction: gaussian (CrysAlis RED; Oxford Diffraction, 2008)	k = −17→17
T_min = 0.209, T_max = 0.623	l = −18→18
38326 measured reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/[σ²(I) + 0.0025I²]
R[F² > 2σ(F²)] = 0.023	(Δ/σ)_max = 0.048
wR(F²) = 0.068	Δρ_max = 1.05 e Å⁻³
S = 1.02	Δρ_min = −0.53 e Å⁻³
7574 reflections	Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
219 parameters	Extinction coefficient: 2863
H-atom parameters constrained

Crystal data top

(C₁₂H₂₈N)₂[Cu_3.194I₆(C₅H₅N)₂]	γ = 81.4137 (18)°
M_r = 1495.3	V = 1198.74 (5) Å³
Triclinic, P1	Z = 1
a = 8.8974 (2) Å	Mo Kα radiation
b = 11.8076 (3) Å	µ = 5.29 mm⁻¹
c = 12.2176 (2) Å	T = 100 K
α = 73.2442 (18)°	0.47 × 0.17 × 0.13 mm
β = 78.5398 (17)°

Data collection top

Oxford Diffraction Xcalibur3 diffractometer with a Sapphire-3 CCD detector	7574 independent reflections
Absorption correction: gaussian (CrysAlis RED; Oxford Diffraction, 2008)	6526 reflections with I > 3σ(I)
T_min = 0.209, T_max = 0.623	R_int = 0.020
38326 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	219 parameters
wR(F²) = 0.068	H-atom parameters constrained
S = 1.02	Δρ_max = 1.05 e Å⁻³
7574 reflections	Δρ_min = −0.53 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
I1	0.975221 (18)	0.302248 (12)	0.020355 (12)	0.01742 (5)
I2	0.969321 (19)	0.432391 (12)	0.321865 (12)	0.01872 (5)
I3	1.283574 (19)	0.118445 (12)	0.272365 (13)	0.01893 (5)
Cu1	1.07925 (4)	0.28339 (3)	0.20757 (2)	0.01739 (9)
Cu2	0.91317 (6)	0.49932 (4)	0.10844 (4)	0.01871 (17)	0.5968 (16)
N1a	0.8219 (2)	0.88100 (15)	0.30754 (15)	0.0131 (5)
C11	0.7234 (3)	0.96480 (18)	0.37333 (18)	0.0144 (6)
C12	0.7803 (3)	1.0861 (2)	0.3507 (2)	0.0222 (8)
C13	0.6638 (3)	1.1587 (2)	0.42004 (19)	0.0194 (7)
C21	0.7404 (3)	0.76914 (19)	0.33556 (19)	0.0154 (6)
C22	0.7369 (3)	0.69023 (19)	0.45874 (19)	0.0171 (7)
C23	0.6214 (3)	0.5995 (2)	0.4812 (2)	0.0210 (7)
C31	0.9801 (3)	0.85294 (18)	0.34363 (18)	0.0149 (6)
C32	1.0882 (3)	0.7620 (2)	0.29315 (19)	0.0174 (7)
C33	1.2416 (3)	0.7437 (2)	0.3369 (2)	0.0212 (8)
C41	0.8411 (3)	0.93675 (19)	0.17762 (17)	0.0155 (6)
C42	0.6926 (3)	0.9801 (3)	0.1284 (2)	0.0278 (9)
C43	0.7306 (3)	1.0288 (2)	−0.0044 (2)	0.0243 (8)
N2p	0.6819 (3)	0.53437 (19)	0.11898 (18)	0.0230 (7)
C1p	0.6020 (4)	0.4452 (2)	0.1892 (2)	0.0280 (9)
C2p	0.4469 (4)	0.4472 (2)	0.1989 (2)	0.0281 (9)
C3p	0.3675 (3)	0.5463 (3)	0.1331 (2)	0.0286 (9)
C4p	0.4470 (3)	0.6379 (2)	0.0616 (2)	0.0255 (8)
C5p	0.6058 (3)	0.6306 (2)	0.0556 (2)	0.0230 (8)
H111	0.709622	0.924955	0.458341	0.0172*
H112	0.615337	0.975346	0.357609	0.0172*
H121	0.788888	1.127677	0.266172	0.0267*
H122	0.882603	1.075863	0.37637	0.0267*
H131	0.700703	1.238077	0.407604	0.0233*
H132	0.561853	1.169742	0.393671	0.0233*
H133	0.652506	1.115708	0.504295	0.0233*
H211	0.632751	0.791309	0.318782	0.0184*
H212	0.788247	0.721678	0.279421	0.0184*
H221	0.704259	0.740092	0.514669	0.0206*
H222	0.841604	0.647834	0.467763	0.0206*
H231	0.630117	0.539099	0.556794	0.0252*
H232	0.514642	0.640855	0.484102	0.0252*
H233	0.643691	0.559055	0.417381	0.0252*
H311	1.030484	0.928078	0.324356	0.0178*
H312	0.968261	0.826734	0.430099	0.0178*
H321	1.106057	0.790999	0.206662	0.0209*
H322	1.041211	0.684915	0.317545	0.0209*
H331	1.307175	0.675529	0.313024	0.0255*
H332	1.295805	0.817379	0.303006	0.0255*
H333	1.222332	0.726026	0.423343	0.0255*
H411	0.904564	0.879347	0.136488	0.0186*
H412	0.907379	1.003709	0.156362	0.0186*
H421	0.627616	0.912646	0.147852	0.0334*
H422	0.635112	1.044646	0.162693	0.0334*
H431	0.635019	1.06992	−0.035239	0.0292*
H432	0.809874	1.086453	−0.024139	0.0292*
H433	0.771582	0.96156	−0.039839	0.0292*
H1p	0.659276	0.374425	0.236251	0.0336*
H2p	0.391005	0.379349	0.251916	0.0337*
H3p	0.253328	0.550155	0.13809	0.0343*
H4p	0.391506	0.709479	0.014187	0.0306*
H5p	0.664306	0.697485	0.003719	0.0276*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
I1	0.01901 (9)	0.01857 (7)	0.01591 (7)	−0.00176 (5)	−0.00510 (6)	−0.00505 (5)
I2	0.02250 (10)	0.01667 (7)	0.01748 (7)	0.00238 (5)	−0.00558 (6)	−0.00593 (5)
I3	0.02042 (9)	0.01691 (7)	0.02043 (7)	0.00264 (5)	−0.00814 (6)	−0.00554 (5)
Cu1	0.01693 (16)	0.01716 (12)	0.01845 (13)	0.00008 (10)	−0.00438 (11)	−0.00525 (10)
Cu2	0.0160 (3)	0.0189 (2)	0.0195 (2)	−0.00081 (17)	−0.00471 (19)	−0.00163 (17)
N1a	0.0134 (10)	0.0132 (7)	0.0128 (7)	−0.0025 (6)	−0.0018 (7)	−0.0032 (6)
C11	0.0146 (11)	0.0147 (8)	0.0134 (8)	−0.0022 (7)	0.0012 (7)	−0.0050 (7)
C12	0.0211 (14)	0.0141 (9)	0.0298 (12)	−0.0046 (8)	0.0039 (10)	−0.0074 (8)
C13	0.0239 (14)	0.0161 (9)	0.0188 (10)	−0.0013 (8)	−0.0012 (9)	−0.0073 (8)
C21	0.0153 (12)	0.0148 (9)	0.0177 (9)	−0.0054 (8)	−0.0026 (8)	−0.0051 (7)
C22	0.0209 (13)	0.0135 (9)	0.0175 (9)	−0.0043 (8)	−0.0041 (8)	−0.0029 (7)
C23	0.0192 (13)	0.0158 (9)	0.0261 (11)	−0.0068 (8)	0.0024 (9)	−0.0042 (8)
C31	0.0155 (12)	0.0140 (8)	0.0172 (9)	−0.0009 (7)	−0.0053 (8)	−0.0059 (7)
C32	0.0170 (12)	0.0184 (9)	0.0186 (9)	−0.0001 (8)	−0.0039 (8)	−0.0077 (8)
C33	0.0175 (13)	0.0243 (11)	0.0256 (11)	0.0025 (9)	−0.0080 (9)	−0.0116 (9)
C41	0.0157 (12)	0.0179 (9)	0.0112 (8)	−0.0010 (8)	−0.0006 (8)	−0.0027 (7)
C42	0.0184 (14)	0.0397 (14)	0.0193 (11)	0.0019 (11)	−0.0043 (10)	−0.0001 (10)
C43	0.0270 (15)	0.0276 (12)	0.0154 (10)	−0.0001 (10)	−0.0048 (9)	−0.0014 (8)
N2p	0.0187 (12)	0.0265 (10)	0.0237 (10)	0.0039 (8)	−0.0079 (8)	−0.0065 (8)
C1p	0.0368 (17)	0.0232 (11)	0.0230 (11)	0.0038 (10)	−0.0124 (11)	−0.0030 (9)
C2p	0.0383 (17)	0.0261 (12)	0.0217 (11)	−0.0126 (11)	−0.0096 (11)	−0.0013 (9)
C3p	0.0220 (15)	0.0369 (14)	0.0267 (12)	−0.0053 (11)	−0.0081 (11)	−0.0042 (10)
C4p	0.0203 (14)	0.0252 (11)	0.0268 (12)	0.0051 (9)	−0.0068 (10)	−0.0022 (9)
C5p	0.0184 (13)	0.0252 (11)	0.0238 (11)	0.0023 (9)	−0.0056 (10)	−0.0047 (9)

Geometric parameters (Å, º) top

I1—Cu1	2.5737 (4)	C31—C32	1.515 (3)
I1—Cu2	2.7752 (6)	C31—H311	1.000
I2—Cu1	2.5223 (3)	C31—H312	1.000
I2—Cu2	2.6239 (5)	C32—C33	1.526 (4)
I3—Cu1	2.5200 (3)	C32—H321	1.000
Cu1—Cu2	2.8208 (5)	C32—H322	1.000
Cu2—N2p	2.023 (2)	C33—H331	1.000
N1a—C11	1.521 (3)	C33—H332	1.000
N1a—C21	1.521 (3)	C33—H333	1.000
N1a—C31	1.520 (3)	C41—C42	1.518 (4)
N1a—C41	1.518 (3)	C41—H411	1.000
C11—C12	1.522 (3)	C41—H412	1.000
C11—H111	1.000	C42—C43	1.542 (3)
C11—H112	1.000	C42—H421	1.000
C12—C13	1.527 (4)	C42—H422	1.000
C12—H121	1.000	C43—H431	1.000
C12—H122	1.000	C43—H432	1.000
C13—H131	1.000	C43—H433	1.000
C13—H132	1.000	N2p—C1p	1.345 (3)
C13—H133	1.000	N2p—C5p	1.349 (3)
C21—C22	1.522 (3)	C1p—C2p	1.359 (5)
C21—H211	1.000	C1p—H1p	1.000
C21—H212	1.000	C2p—C3p	1.398 (4)
C22—C23	1.525 (4)	C2p—H2p	1.000
C22—H221	1.000	C3p—C4p	1.368 (4)
C22—H222	1.000	C3p—H3p	1.000
C23—H231	1.000	C4p—C5p	1.391 (4)
C23—H232	1.000	C4p—H4p	1.000
C23—H233	1.000	C5p—H5p	1.000

Cu1—I1—Cu2	63.521 (13)	C22—C23—H233	109.5
Cu1—I2—Cu2	66.443 (13)	H231—C23—H232	109.5
I1—Cu1—I2	118.078 (12)	H231—C23—H233	109.5
I1—Cu1—I3	119.911 (13)	H232—C23—H233	109.5
I1—Cu1—Cu2	61.722 (14)	N1a—C31—C32	115.7 (2)
I2—Cu1—I3	122.009 (14)	N1a—C31—H311	109.47
I2—Cu1—Cu2	58.506 (13)	N1a—C31—H312	109.47
I3—Cu1—Cu2	165.993 (17)	C32—C31—H311	109.47
I1—Cu2—I2	108.039 (16)	C32—C31—H312	109.47
I1—Cu2—Cu1	54.757 (12)	H311—C31—H312	102.4
I1—Cu2—N2p	102.85 (8)	C31—C32—C33	109.6 (2)
I1ⁱ—Cu2—I1	117.966 (18)	C31—C32—H321	109.47
I1ⁱ—Cu2—I2	115.09 (2)	C31—C32—H322	109.5
I1ⁱ—Cu2—Cu1	127.61 (2)	C33—C32—H321	109.5
I1ⁱ—Cu2—Cu2ⁱ	61.601 (15)	C33—C32—H322	109.47
I1ⁱ—Cu2—N2p	104.91 (6)	H321—C32—H322	109.4
I1ⁱ—Cu2—C1p	130.33 (5)	C32—C33—H331	109.5
I1ⁱ—Cu2—H1p	149.99 (2)	C32—C33—H332	109.5
I2—Cu2—Cu1	55.051 (12)	C32—C33—H333	109.5
I2—Cu2—Cu2ⁱ	135.09 (2)	H331—C33—H332	109.5
I2—Cu2—N2p	106.60 (6)	H331—C33—H333	109.5
Cu1—Cu2—N2p	127.48 (6)	H332—C33—H333	109.5
C11—N1a—C21	107.99 (16)	N1a—C41—C42	115.60 (18)
C11—N1a—C31	109.17 (19)	N1a—C41—H411	109.47
C11—N1a—C41	111.12 (15)	N1a—C41—H412	109.5
C21—N1a—C31	111.36 (15)	C42—C41—H411	109.5
C21—N1a—C41	108.49 (19)	C42—C41—H412	109.47
C31—N1a—C41	108.72 (16)	H411—C41—H412	102.6
N1a—C11—C12	116.13 (18)	C41—C42—C43	109.5 (2)
N1a—C11—H111	109.47	C41—C42—H421	109.5
C12—C11—H112	109.47	C41—C42—H422	109.5
H111—C11—H112	101.87	C43—C42—H421	109.5
C11—C12—C13	108.40 (19)	C43—C42—H422	109.5
C11—C12—H121	109.5	H421—C42—H422	109.4
C11—C12—H122	109.47	C42—C43—H431	109.5
C13—C12—H121	109.47	C42—C43—H432	109.5
C13—C12—H122	109.5	C42—C43—H433	109.5
H121—C12—H122	110.5	H431—C43—H432	109.5
C12—C13—H131	109.5	H431—C43—H433	109.5
C12—C13—H132	109.5	H432—C43—H433	109.5
C12—C13—H133	109.47	Cu2—N2p—C1p	114.07 (17)
H131—C13—H132	109.5	Cu2—N2p—C5p	126.45 (17)
H131—C13—H133	109.5	C1p—N2p—C5p	119.2 (2)
H132—C13—H133	109.5	N2p—C1p—C2p	122.8 (2)
N1a—C21—C22	115.4 (2)	N2p—C1p—H1p	118.6
N1a—C21—H211	109.47	C2p—C1p—H1p	118.6
N1a—C21—H212	109.47	C1p—C2p—C3p	118.4 (2)
C22—C21—H211	109.47	C1p—C2p—H2p	120.8
C22—C21—H212	109.47	C3p—C2p—H2p	120.8
H211—C21—H212	102.9	C2p—C3p—C4p	119.5 (3)
C21—C22—C23	108.7 (2)	C2p—C3p—H3p	120.2
C21—C22—H221	109.47	C4p—C3p—H3p	120.2
C21—C22—H222	109.47	C3p—C4p—C5p	119.3 (2)
C23—C22—H221	109.5	C3p—C4p—H4p	120.3
C23—C22—H222	109.47	C5p—C4p—H4p	120.3
H221—C22—H222	110.3	N2p—C5p—C4p	120.8 (2)
C22—C23—H231	109.5	N2p—C5p—H5p	119.6
C22—C23—H232	109.5	C4p—C5p—H5p	119.6

Symmetry code: (i) −x+2, −y+1, −z.

Experimental details

Crystal data
Chemical formula	(C₁₂H₂₈N)₂[Cu_3.194I₆(C₅H₅N)₂]
M_r	1495.3
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	8.8974 (2), 11.8076 (3), 12.2176 (2)
α, β, γ (°)	73.2442 (18), 78.5398 (17), 81.4137 (18)
V (Å³)	1198.74 (5)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	5.29
Crystal size (mm)	0.47 × 0.17 × 0.13

Data collection
Diffractometer	Oxford Diffraction Xcalibur3 diffractometer with a Sapphire-3 CCD detector
Absorption correction	Gaussian (CrysAlis RED; Oxford Diffraction, 2008)
T_min, T_max	0.209, 0.623
No. of measured, independent and observed [I > 3σ(I)] reflections	38326, 7574, 6526
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.750

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.068, 1.02
No. of reflections	7574
No. of parameters	219
No. of restraints	?
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.05, −0.53

Computer programs: CrysAlis CCD (Oxford Diffraction, 2008), CrysAlis RED (Oxford Diffraction, 2008), SUPERFLIP (Oszlányi & Sütő, 2004), JANA2000 (Petricek et al., 2000), DIAMOND (Brandenburg, 1999).

Acknowledgements

Financial support from the Swedish Research Council is gratefully acknowledged

References

Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147. CrossRef IUCr Journals Web of Science Google Scholar
Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Cariati, E., Roberto, D., Ugo, R., Ford, P. C., Galli, S. & Sironi, A. (2005). Inorg. Chem. 44, 4077–4085. Web of Science CSD CrossRef PubMed CAS Google Scholar
Oszlányi, G. & Sütő, A. (2004). Acta Cryst. A60, 134–141. Web of Science CrossRef IUCr Journals Google Scholar
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England. Google Scholar
Petříček, V., Dušek, M. & Palatinus, L. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Google Scholar

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