Bis­(tetraethyl­ammonium) μ-tetra­thio­molybdato(VI)-bis­[chloro­copper(I)]

The title compound, (Et₄N)₂[MoS₄(CuCl)₂], consists of tetraethyl­ammonium cations of expected geometry, and trinuclear anions in which two opposite edges of an MoS₄²⁻ tetrahedron are bridged by CuCl units. The bridging of Mo and Cu centres by all four S atoms hardly affects the tetrahedral coordination of Mo and leads to a distorted trigonal planar coordination geometry for Cu, with both chloro ligands terminal.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.033
• wR factor = 0.071
• Data-to-parameter ratio = 19.2

checkCIF/PLATON results

No syntax errors found



Alert level C
CRYSC01_ALERT_1_C The word below has not been recognised as a standard
            identifier.
            deep
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.99
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?

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

   2 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

(I)

Crystal data

(C8H20N)2[CuMoCl2S4]	F(000) = 1392
Mr = 682.66	Dx = 1.634 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 7.5052 (5) Å	Cell parameters from 1000 reflections
b = 13.2537 (9) Å	θ = 2.5–25.0°
c = 27.9439 (18) Å	µ = 2.46 mm^−1
β = 93.175 (1)°	T = 150 K
V = 2775.4 (3) Å^3	Block, deep violet
Z = 4	0.18 × 0.12 × 0.10 mm

Data collection

Bruker SMART 1K CCD diffractometer	4845 independent reflections
Radiation source: sealed tube	3525 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.048
Detector resolution: 8.192 pixels mm^-1	θmax = 25.0°, θmin = 1.7°
thin–slice ω scans	h = −8→8
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	k = −15→15
Tmin = 0.698, Tmax = 0.782	l = −33→30
15663 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.071	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0256P)^2 + 0.3229P] where P = (Fo^2 + 2Fc^2)/3
4845 reflections	(Δ/σ)max = 0.001
252 parameters	Δρmax = 0.43 e Å^−3
0 restraints	Δρmin = −0.47 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Mo	0.72508 (4)	0.25634 (2)	0.381231 (12)	0.02045 (10)
Cu1	0.56140 (6)	0.08216 (3)	0.373848 (17)	0.02707 (14)
Cu2	0.89008 (6)	0.42862 (3)	0.384924 (17)	0.02569 (14)
S1	0.55509 (15)	0.20339 (8)	0.31914 (4)	0.0347 (3)
S2	0.73087 (14)	0.13609 (7)	0.43647 (4)	0.0251 (2)
S3	0.99908 (14)	0.28471 (8)	0.35867 (4)	0.0280 (3)
S4	0.61835 (14)	0.39940 (7)	0.40902 (4)	0.0296 (3)
Cl1	0.43352 (15)	−0.06386 (7)	0.36616 (4)	0.0364 (3)
Cl2	1.01851 (13)	0.57431 (7)	0.38449 (4)	0.0301 (3)
N1	0.4477 (4)	0.5840 (2)	0.27277 (11)	0.0192 (7)
C1	0.3390 (5)	0.5020 (3)	0.29519 (14)	0.0268 (10)
H1A	0.4173	0.4430	0.3019	0.032*
H1B	0.2996	0.5269	0.3263	0.032*
C2	0.1763 (6)	0.4674 (3)	0.26512 (16)	0.0389 (12)
H2A	0.0905	0.5229	0.2616	0.058*
H2B	0.1210	0.4102	0.2809	0.058*
H2C	0.2123	0.4466	0.2334	0.058*
C3	0.5335 (6)	0.5457 (3)	0.22805 (15)	0.0314 (11)
H3A	0.4376	0.5237	0.2046	0.038*
H3B	0.5969	0.6025	0.2135	0.038*
C4	0.6637 (6)	0.4593 (3)	0.23616 (18)	0.0504 (14)
H4A	0.7607	0.4801	0.2589	0.076*
H4B	0.7131	0.4405	0.2057	0.076*
H4C	0.6016	0.4012	0.2491	0.076*
C5	0.5842 (5)	0.6179 (3)	0.31048 (15)	0.0315 (10)
H5A	0.6634	0.5601	0.3190	0.038*
H5B	0.5219	0.6364	0.3395	0.038*
C6	0.6987 (6)	0.7058 (3)	0.29697 (17)	0.0448 (13)
H6A	0.7504	0.6919	0.2662	0.067*
H6B	0.7948	0.7156	0.3217	0.067*
H6C	0.6254	0.7669	0.2942	0.067*
C7	0.3310 (5)	0.6709 (3)	0.25623 (14)	0.0242 (9)
H7A	0.2436	0.6461	0.2311	0.029*
H7B	0.4066	0.7219	0.2413	0.029*
C8	0.2297 (6)	0.7224 (3)	0.29467 (16)	0.0366 (11)
H8A	0.1591	0.6723	0.3111	0.055*
H8B	0.1500	0.7736	0.2799	0.055*
H8C	0.3144	0.7547	0.3178	0.055*
N2	0.2560 (4)	0.2288 (2)	0.52346 (11)	0.0203 (7)
C9	0.2444 (6)	0.2956 (3)	0.47963 (14)	0.0308 (10)
H9A	0.1572	0.2658	0.4558	0.037*
H9B	0.3621	0.2959	0.4653	0.037*
C10	0.1900 (7)	0.4045 (3)	0.48891 (16)	0.0456 (13)
H10A	0.0693	0.4057	0.5006	0.068*
H10B	0.1921	0.4432	0.4591	0.068*
H10C	0.2737	0.4345	0.5130	0.068*
C11	0.3741 (5)	0.2764 (3)	0.56354 (14)	0.0242 (9)
H11A	0.3135	0.3375	0.5750	0.029*
H11B	0.3856	0.2283	0.5906	0.029*
C12	0.5603 (5)	0.3059 (3)	0.54972 (15)	0.0381 (11)
H12A	0.6227	0.2460	0.5387	0.057*
H12B	0.6270	0.3346	0.5776	0.057*
H12C	0.5512	0.3561	0.5240	0.057*
C13	0.0702 (5)	0.2142 (3)	0.54106 (14)	0.0266 (10)
H13A	0.0243	0.2807	0.5508	0.032*
H13B	−0.0087	0.1897	0.5140	0.032*
C14	0.0568 (5)	0.1419 (3)	0.58253 (15)	0.0348 (11)
H14A	0.0941	0.0744	0.5728	0.052*
H14B	−0.0669	0.1393	0.5920	0.052*
H14C	0.1344	0.1650	0.6097	0.052*
C15	0.3371 (5)	0.1288 (3)	0.51008 (14)	0.0248 (10)
H15A	0.4575	0.1415	0.4986	0.030*
H15B	0.3519	0.0867	0.5393	0.030*
C16	0.2310 (5)	0.0699 (3)	0.47231 (15)	0.0319 (11)
H16A	0.1135	0.0537	0.4839	0.048*
H16B	0.2942	0.0073	0.4654	0.048*
H16C	0.2162	0.1104	0.4430	0.048*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo	0.02160 (19)	0.02293 (19)	0.01668 (19)	−0.00241 (15)	−0.00021 (14)	−0.00022 (15)
Cu1	0.0290 (3)	0.0268 (3)	0.0252 (3)	−0.0060 (2)	0.0006 (2)	−0.0031 (2)
Cu2	0.0291 (3)	0.0247 (3)	0.0234 (3)	−0.0047 (2)	0.0021 (2)	−0.0003 (2)
S1	0.0365 (7)	0.0428 (7)	0.0236 (6)	−0.0131 (5)	−0.0090 (5)	0.0048 (5)
S2	0.0290 (6)	0.0254 (5)	0.0206 (6)	−0.0015 (4)	−0.0015 (5)	0.0016 (4)
S3	0.0274 (6)	0.0299 (6)	0.0272 (6)	−0.0040 (5)	0.0071 (5)	−0.0065 (5)
S4	0.0281 (6)	0.0252 (5)	0.0364 (7)	0.0019 (5)	0.0084 (5)	0.0016 (5)
Cl1	0.0466 (7)	0.0293 (6)	0.0325 (7)	−0.0120 (5)	−0.0047 (5)	−0.0035 (5)
Cl2	0.0337 (6)	0.0251 (5)	0.0324 (6)	−0.0043 (4)	0.0096 (5)	−0.0036 (4)
N1	0.0177 (17)	0.0218 (17)	0.0180 (18)	−0.0014 (14)	0.0004 (14)	0.0027 (14)
C1	0.029 (2)	0.022 (2)	0.030 (3)	−0.0007 (18)	0.008 (2)	0.0035 (18)
C2	0.049 (3)	0.032 (2)	0.036 (3)	−0.014 (2)	0.005 (2)	−0.003 (2)
C3	0.036 (3)	0.033 (2)	0.026 (3)	−0.006 (2)	0.014 (2)	−0.001 (2)
C4	0.048 (3)	0.033 (3)	0.073 (4)	0.008 (2)	0.032 (3)	0.000 (3)
C5	0.025 (2)	0.040 (3)	0.029 (3)	−0.007 (2)	−0.007 (2)	−0.002 (2)
C6	0.031 (3)	0.056 (3)	0.047 (3)	−0.015 (2)	−0.002 (2)	−0.002 (3)
C7	0.027 (2)	0.020 (2)	0.026 (2)	0.0002 (18)	−0.0044 (19)	0.0055 (18)
C8	0.032 (3)	0.025 (2)	0.054 (3)	−0.001 (2)	0.007 (2)	−0.006 (2)
N2	0.0197 (18)	0.0241 (17)	0.0169 (18)	−0.0005 (14)	0.0006 (14)	−0.0021 (14)
C9	0.044 (3)	0.031 (2)	0.017 (2)	0.000 (2)	−0.004 (2)	0.0032 (19)
C10	0.069 (4)	0.034 (3)	0.032 (3)	0.005 (2)	−0.007 (3)	0.008 (2)
C11	0.024 (2)	0.026 (2)	0.022 (2)	−0.0065 (18)	−0.0036 (18)	−0.0029 (18)
C12	0.030 (3)	0.055 (3)	0.029 (3)	−0.012 (2)	−0.002 (2)	−0.005 (2)
C13	0.018 (2)	0.031 (2)	0.031 (3)	−0.0010 (18)	0.0067 (19)	−0.0123 (19)
C14	0.028 (3)	0.038 (3)	0.039 (3)	−0.010 (2)	0.011 (2)	−0.010 (2)
C15	0.023 (2)	0.025 (2)	0.027 (2)	0.0029 (18)	0.0056 (19)	−0.0018 (18)
C16	0.034 (3)	0.030 (2)	0.032 (3)	0.001 (2)	0.003 (2)	−0.013 (2)

Geometric parameters (Å, º)

Mo—Cu1	2.6178 (6)	C7—H7A	0.990
Mo—Cu2	2.5969 (6)	C7—H7B	0.990
Mo—S1	2.2102 (11)	C7—C8	1.512 (5)
Mo—S2	2.2174 (10)	C8—H8A	0.980
Mo—S3	2.2162 (11)	C8—H8B	0.980
Mo—S4	2.2156 (10)	C8—H8C	0.980
Cu1—S1	2.2165 (12)	N2—C9	1.510 (5)
Cu1—S2	2.2235 (11)	N2—C11	1.526 (5)
Cu1—Cl1	2.1656 (11)	N2—C13	1.517 (4)
Cu2—S3	2.2163 (11)	N2—C15	1.515 (4)
Cu2—S4	2.2169 (11)	C9—H9A	0.990
Cu2—Cl2	2.1584 (10)	C9—H9B	0.990
N1—C1	1.516 (4)	C9—C10	1.526 (5)
N1—C3	1.525 (5)	C10—H10A	0.980
N1—C5	1.497 (5)	C10—H10B	0.980
N1—C7	1.504 (4)	C10—H10C	0.980
C1—H1A	0.990	C11—H11A	0.990
C1—H1B	0.990	C11—H11B	0.990
C1—C2	1.514 (6)	C11—C12	1.521 (5)
C2—H2A	0.980	C12—H12A	0.980
C2—H2B	0.980	C12—H12B	0.980
C2—H2C	0.980	C12—H12C	0.980
C3—H3A	0.990	C13—H13A	0.990
C3—H3B	0.990	C13—H13B	0.990
C3—C4	1.514 (5)	C13—C14	1.512 (5)
C4—H4A	0.980	C14—H14A	0.980
C4—H4B	0.980	C14—H14B	0.980
C4—H4C	0.980	C14—H14C	0.980
C5—H5A	0.990	C15—H15A	0.990
C5—H5B	0.990	C15—H15B	0.990
C5—C6	1.508 (5)	C15—C16	1.505 (5)
C6—H6A	0.980	C16—H16A	0.980
C6—H6B	0.980	C16—H16B	0.980
C6—H6C	0.980	C16—H16C	0.980
S1—Mo—S2	107.84 (4)	H7A—C7—C8	108.3
S1—Mo—S3	109.57 (4)	H7B—C7—C8	108.3
S1—Mo—S4	110.04 (5)	C7—C8—H8A	109.5
S2—Mo—S3	109.71 (4)	C7—C8—H8B	109.5
S2—Mo—S4	111.38 (4)	C7—C8—H8C	109.5
S3—Mo—S4	108.28 (4)	H8A—C8—H8B	109.5
S1—Cu1—S2	107.41 (4)	H8A—C8—H8C	109.5
S1—Cu1—Cl1	125.94 (5)	H8B—C8—H8C	109.5
S2—Cu1—Cl1	126.61 (4)	C9—N2—C11	111.0 (3)
S3—Cu2—S4	108.23 (4)	C9—N2—C13	109.0 (3)
S3—Cu2—Cl2	126.51 (4)	C9—N2—C15	108.6 (3)
S4—Cu2—Cl2	125.21 (4)	C11—N2—C13	108.8 (3)
Mo—S1—Cu1	72.51 (4)	C11—N2—C15	108.6 (3)
Mo—S2—Cu1	72.24 (3)	C13—N2—C15	110.9 (3)
Mo—S3—Cu2	71.73 (3)	N2—C9—H9A	108.6
Mo—S4—Cu2	71.73 (3)	N2—C9—H9B	108.6
C1—N1—C3	111.2 (3)	N2—C9—C10	114.9 (3)
C1—N1—C5	106.7 (3)	H9A—C9—H9B	107.5
C1—N1—C7	111.0 (3)	H9A—C9—C10	108.6
C3—N1—C5	111.9 (3)	H9B—C9—C10	108.6
C3—N1—C7	105.6 (3)	C9—C10—H10A	109.5
C5—N1—C7	110.6 (3)	C9—C10—H10B	109.5
N1—C1—H1A	108.5	C9—C10—H10C	109.5
N1—C1—H1B	108.5	H10A—C10—H10B	109.5
N1—C1—C2	115.1 (3)	H10A—C10—H10C	109.5
H1A—C1—H1B	107.5	H10B—C10—H10C	109.5
H1A—C1—C2	108.5	N2—C11—H11A	108.5
H1B—C1—C2	108.5	N2—C11—H11B	108.5
C1—C2—H2A	109.5	N2—C11—C12	115.1 (3)
C1—C2—H2B	109.5	H11A—C11—H11B	107.5
C1—C2—H2C	109.5	H11A—C11—C12	108.5
H2A—C2—H2B	109.5	H11B—C11—C12	108.5
H2A—C2—H2C	109.5	C11—C12—H12A	109.5
H2B—C2—H2C	109.5	C11—C12—H12B	109.5
N1—C3—H3A	108.4	C11—C12—H12C	109.5
N1—C3—H3B	108.4	H12A—C12—H12B	109.5
N1—C3—C4	115.3 (3)	H12A—C12—H12C	109.5
H3A—C3—H3B	107.5	H12B—C12—H12C	109.5
H3A—C3—C4	108.4	N2—C13—H13A	108.4
H3B—C3—C4	108.4	N2—C13—H13B	108.4
C3—C4—H4A	109.5	N2—C13—C14	115.5 (3)
C3—C4—H4B	109.5	H13A—C13—H13B	107.5
C3—C4—H4C	109.5	H13A—C13—C14	108.4
H4A—C4—H4B	109.5	H13B—C13—C14	108.4
H4A—C4—H4C	109.5	C13—C14—H14A	109.5
H4B—C4—H4C	109.5	C13—C14—H14B	109.5
N1—C5—H5A	108.4	C13—C14—H14C	109.5
N1—C5—H5B	108.4	H14A—C14—H14B	109.5
N1—C5—C6	115.6 (3)	H14A—C14—H14C	109.5
H5A—C5—H5B	107.4	H14B—C14—H14C	109.5
H5A—C5—C6	108.4	N2—C15—H15A	108.5
H5B—C5—C6	108.4	N2—C15—H15B	108.5
C5—C6—H6A	109.5	N2—C15—C16	115.0 (3)
C5—C6—H6B	109.5	H15A—C15—H15B	107.5
C5—C6—H6C	109.5	H15A—C15—C16	108.5
H6A—C6—H6B	109.5	H15B—C15—C16	108.5
H6A—C6—H6C	109.5	C15—C16—H16A	109.5
H6B—C6—H6C	109.5	C15—C16—H16B	109.5
N1—C7—H7A	108.3	C15—C16—H16C	109.5
N1—C7—H7B	108.3	H16A—C16—H16B	109.5
N1—C7—C8	115.7 (3)	H16A—C16—H16C	109.5
H7A—C7—H7B	107.4	H16B—C16—H16C	109.5
S2—Mo—S1—Cu1	−0.41 (4)	C7—N1—C1—C2	51.3 (4)
S3—Mo—S1—Cu1	118.96 (4)	C1—N1—C3—C4	−61.5 (4)
S4—Mo—S1—Cu1	−122.09 (4)	C5—N1—C3—C4	57.6 (4)
S2—Cu1—S1—Mo	0.41 (4)	C7—N1—C3—C4	178.0 (3)
Cl1—Cu1—S1—Mo	−177.50 (5)	C1—N1—C5—C6	−175.3 (3)
S1—Mo—S2—Cu1	0.41 (4)	C3—N1—C5—C6	62.9 (4)
S3—Mo—S2—Cu1	−118.87 (4)	C7—N1—C5—C6	−54.5 (4)
S4—Mo—S2—Cu1	121.25 (4)	C1—N1—C7—C8	59.3 (4)
S1—Cu1—S2—Mo	−0.41 (4)	C3—N1—C7—C8	179.9 (3)
Cl1—Cu1—S2—Mo	177.49 (5)	C5—N1—C7—C8	−58.9 (4)
S1—Mo—S3—Cu2	118.76 (4)	C11—N2—C9—C10	−52.4 (4)
S2—Mo—S3—Cu2	−123.03 (4)	C13—N2—C9—C10	67.3 (4)
S4—Mo—S3—Cu2	−1.27 (5)	C15—N2—C9—C10	−171.7 (3)
S4—Cu2—S3—Mo	1.27 (5)	C9—N2—C11—C12	−54.1 (4)
Cl2—Cu2—S3—Mo	−176.15 (5)	C13—N2—C11—C12	−174.0 (3)
S1—Mo—S4—Cu2	−118.46 (4)	C15—N2—C11—C12	65.2 (4)
S2—Mo—S4—Cu2	121.99 (4)	C9—N2—C13—C14	175.2 (3)
S3—Mo—S4—Cu2	1.27 (5)	C11—N2—C13—C14	−63.7 (4)
S3—Cu2—S4—Mo	−1.27 (5)	C15—N2—C13—C14	55.6 (4)
Cl2—Cu2—S4—Mo	176.20 (5)	C9—N2—C15—C16	−61.9 (4)
C3—N1—C1—C2	−65.9 (4)	C11—N2—C15—C16	177.3 (3)
C5—N1—C1—C2	171.9 (3)	C13—N2—C15—C16	57.9 (4)