Bis(tetra-propyl-ammonium) di-μ(3)-iodido-di-μ(2)-iodido-diiodidodi-pyridine-tetra-copper(I).

The title compound, (C(12)H(28)N)(2)[Cu(3.194)I(6)(C(5)H(5)N)(2)] was prepared from reaction of copper powder, copper(I) oxide, hydro-iodic acid, tetra-propyl-ammonium iodide and pyridine under hydro-thermal conditions. In the centrosymmetric Cu(4)I(6) (2-) 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[Cu3.194I6(C5H5N)2]

M = 1495.3

Triclinic,

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 ▶) 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[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.068

S = 1.02

7574 reflections

219 parameters

H-atom parameters constrained

Δρmax = 1.05 e Å−3

Δρmin = −0.53 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2008 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2008 ▶); 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.

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

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

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C12H28N)2[Cu3.194I6(C5H5N)2]	Z = 1
Mr = 1495.3	F(000) = 708.8
Triclinic, P1	Dx = 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

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	Rint = 0.020
Detector resolution: 16.5467 pixels mm-1	θmax = 32.2°, θmin = 4.3°
ω scans	h = −13→13
Absorption correction: gaussian (CrysAlis RED; Oxford Diffraction, 2008)	k = −17→17
Tmin = 0.209, Tmax = 0.623	l = −18→18
38326 measured reflections

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	Δρmax = 1.05 e Å−3
S = 1.02	Δρmin = −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

	x	y	z	Uiso*/Ueq	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*

	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)

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