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The title compound, bis­(tetra-n-butyl­ammonium) tetra­chloro­tetra-μ3-sulfidotetracopper(I)molybdenum(VI), (C16H36N)2[MoS4(CuCl)4], has been obtained in a second polymorphic form. The anion, in which four of the six S...S edges of the central MoS4 tetrahedron are bridged by CuCl neutral molecular units to give a planar pentanuclear MoCu4 framework, is disordered on a crystallographic fourfold rotation axis, requiring equal occupancy of two sets of four positions for the S atoms. There is additional disorder as a result of 8.2 (2)% substitution of Cl by Br, arising from tetra-n-butyl­ammonium bromide used in the synthesis. Copper has distorted trigonal planar coordination, involving two μ3-S atoms and a terminal halogen atom. The two independent cations lie on positions of symmetry \overline 4.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804001175/bt6400sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804001175/bt6400Isup2.hkl
Contains datablock I

CCDC reference: 234818

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.024
  • wR factor = 0.058
  • Data-to-parameter ratio = 23.5

checkCIF/PLATON results

No syntax errors found



Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR) is > 1.50 Tmin and Tmax reported: 0.701 0.876 Tmin and Tmax expected: 0.363 0.876 RR = 1.932 Please check that your absorption correction is appropriate. PLAT060_ALERT_3_B Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.94
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 10.00 Perc.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 5 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 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: EVALCCD (Duisenberg et al., 2003); data reduction: EVALCCD; 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) top
Crystal data top
(C16H36N)2[MoS4(CuCl)4]Dx = 1.532 Mg m3
Mr = 1119.51Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/nCell parameters from 86 reflections
a = 13.3356 (6) Åθ = 2.5–25.0°
c = 13.6495 (9) ŵ = 2.64 mm1
V = 2427.4 (2) Å3T = 150 K
Z = 2Plate, purple
F(000) = 11480.40 × 0.40 × 0.05 mm
Data collection top
Nonius KappaCCD
diffractometer
2796 independent reflections
Radiation source: sealed tube2191 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
φ and ω scansθmax = 27.5°, θmin = 4.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 1717
Tmin = 0.701, Tmax = 0.876k = 1517
19584 measured reflectionsl = 1717
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0191P)2 + 1.5691P]
where P = (Fo2 + 2Fc2)/3
2796 reflections(Δ/σ)max = 0.001
119 parametersΔρmax = 0.46 e Å3
0 restraintsΔρmin = 0.36 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo0.25000.25000.26798 (2)0.02315 (9)
Cu0.066050 (18)0.319184 (19)0.262395 (18)0.02955 (8)
Cl0.08479 (3)0.37625 (4)0.25092 (3)0.0390 (2)0.918 (2)
Br0.08479 (3)0.37625 (4)0.25092 (3)0.0390 (2)0.082 (2)
S0.19314 (8)0.37513 (9)0.17358 (8)0.0326 (2)0.50
S'0.19175 (8)0.37831 (8)0.35937 (7)0.0287 (2)0.50
N10.75000.25000.00000.0221 (7)
C10.83183 (14)0.28816 (14)0.06781 (13)0.0254 (4)
H1A0.84850.23390.11450.030*
H1B0.80400.34450.10640.030*
C20.92831 (15)0.32343 (15)0.02096 (15)0.0294 (4)
H2A0.96300.26640.01070.035*
H2B0.91380.37450.02970.035*
C30.99475 (17)0.36846 (18)0.10127 (17)0.0394 (5)
H3A1.00030.32000.15590.047*
H3B0.96250.42990.12700.047*
C41.09892 (18)0.39429 (19)0.0651 (2)0.0546 (7)
H4A1.09390.44050.00950.082*
H4B1.13700.42620.11810.082*
H4C1.13330.33290.04440.082*
N20.75000.25000.50000.0243 (7)
C50.82834 (15)0.29530 (15)0.56782 (14)0.0273 (4)
H5A0.79410.34220.61300.033*
H5B0.85730.24070.60800.033*
C60.91377 (16)0.35107 (18)0.51841 (16)0.0383 (5)
H6A0.88740.41160.48520.046*
H6B0.94510.30750.46830.046*
C70.99263 (18)0.38174 (17)0.59482 (18)0.0411 (6)
H7A1.03660.43380.56600.049*
H7B0.95800.41190.65180.049*
C81.05661 (19)0.2959 (2)0.62988 (19)0.0497 (7)
H8A1.01390.24490.66040.075*
H8B1.10530.32060.67790.075*
H8C1.09230.26640.57410.075*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo0.02494 (12)0.02494 (12)0.01956 (16)0.0000.0000.000
Cu0.02496 (14)0.03581 (15)0.02788 (14)0.00148 (11)0.00074 (10)0.00147 (11)
Cl0.0252 (3)0.0633 (4)0.0286 (3)0.0060 (2)0.00074 (18)0.0018 (2)
Br0.0252 (3)0.0633 (4)0.0286 (3)0.0060 (2)0.00074 (18)0.0018 (2)
S0.0252 (5)0.0437 (6)0.0290 (5)0.0016 (5)0.0023 (4)0.0128 (5)
S'0.0285 (5)0.0318 (6)0.0259 (5)0.0023 (4)0.0028 (4)0.0072 (4)
N10.0235 (10)0.0235 (10)0.0192 (15)0.0000.0000.000
C10.0296 (11)0.0239 (10)0.0225 (9)0.0005 (8)0.0054 (8)0.0008 (8)
C20.0299 (11)0.0280 (11)0.0305 (10)0.0010 (9)0.0065 (9)0.0008 (8)
C30.0387 (13)0.0354 (13)0.0442 (13)0.0028 (10)0.0155 (10)0.0022 (10)
C40.0377 (14)0.0411 (14)0.085 (2)0.0092 (11)0.0174 (14)0.0015 (14)
N20.0258 (11)0.0258 (11)0.0213 (16)0.0000.0000.000
C50.0301 (11)0.0278 (11)0.0240 (9)0.0025 (8)0.0051 (8)0.0001 (8)
C60.0377 (13)0.0427 (13)0.0345 (11)0.0124 (10)0.0078 (10)0.0089 (10)
C70.0422 (14)0.0384 (13)0.0428 (13)0.0135 (11)0.0107 (11)0.0037 (10)
C80.0412 (14)0.0592 (17)0.0487 (15)0.0090 (12)0.0086 (11)0.0062 (13)
Geometric parameters (Å, º) top
Mo—Cu2.6220 (3)C2—H2B0.990
Mo—Cui2.6220 (3)C2—C31.532 (3)
Mo—Cuii2.6220 (3)C3—H3A0.990
Mo—Cuiii2.6220 (3)C3—H3B0.990
Mo—S2.2406 (10)C3—C41.514 (3)
Mo—Si2.2406 (10)C4—H4A0.980
Mo—Sii2.2406 (10)C4—H4B0.980
Mo—Siii2.2406 (10)C4—H4C0.980
Mo—S'2.2556 (10)N2—C51.5210 (18)
Mo—S'i2.2556 (10)N2—C5iv1.5210 (18)
Mo—S'iii2.2556 (10)N2—C5vii1.5210 (18)
Mo—S'ii2.2556 (10)N2—C5viii1.5210 (18)
Cu—Cl2.1563 (5)C5—H5A0.990
Cu—S2.2134 (10)C5—H5B0.990
Cu—Sii2.2159 (11)C5—C61.519 (3)
Cu—S'2.2768 (10)C6—H6A0.990
Cu—S'ii2.2783 (10)C6—H6B0.990
N1—C11.5187 (18)C6—C71.536 (3)
N1—C1iv1.5187 (18)C7—H7A0.990
N1—C1v1.5187 (18)C7—H7B0.990
N1—C1vi1.5187 (18)C7—C81.505 (3)
C1—H1A0.990C8—H8A0.980
C1—H1B0.990C8—H8B0.980
C1—C21.512 (3)C8—H8C0.980
C2—H2A0.990
Sii—Mo—Siii109.78 (6)C2—C3—H3A109.0
S—Mo—Si109.78 (6)C2—C3—H3B109.0
Si—Mo—S'iii108.53 (4)C2—C3—C4112.7 (2)
S—Mo—S'iii108.56 (4)H3A—C3—H3B107.8
Sii—Mo—S'108.56 (4)H3A—C3—C4109.0
Siii—Mo—S'108.53 (4)H3B—C3—C4109.0
Si—Mo—S'ii108.56 (4)C3—C4—H4A109.5
S—Mo—S'ii108.53 (4)C3—C4—H4B109.5
Sii—Mo—S'i108.53 (4)C3—C4—H4C109.5
Siii—Mo—S'i108.56 (4)H4A—C4—H4B109.5
S'iii—Mo—S'ii112.85 (5)H4A—C4—H4C109.5
S'—Mo—S'i112.85 (5)H4B—C4—H4C109.5
Cl—Cu—S123.75 (3)C5—N2—C5vii111.74 (8)
Cl—Cu—Sii123.93 (3)C5—N2—C5viii111.74 (8)
Cl—Cu—S'127.36 (3)C5vii—N2—C5viii105.02 (15)
Cl—Cu—S'ii127.53 (3)C5—N2—C5iv105.02 (15)
Sii—Cu—S'108.67 (4)C5vii—N2—C5iv111.74 (8)
S—Cu—S'ii108.68 (4)C5viii—N2—C5iv111.74 (8)
Mo—S—Cu72.12 (3)N2—C5—H5A108.3
Mo—S—Cuiii72.08 (3)N2—C5—H5B108.3
Cu—S—Cuiii113.61 (5)N2—C5—C6116.08 (15)
Mo—S'—Cu70.69 (3)H5A—C5—H5B107.4
Mo—S'—Cuiii70.66 (3)H5A—C5—C6108.3
Cu—S'—Cuiii108.91 (4)H5B—C5—C6108.3
C1iv—N1—C1vi111.81 (8)C5—C6—H6A109.7
C1—N1—C1iv104.90 (14)C5—C6—H6B109.7
C1—N1—C1vi111.81 (8)C5—C6—C7110.02 (18)
C1iv—N1—C1v111.81 (8)H6A—C6—H6B108.2
C1vi—N1—C1v104.90 (14)H6A—C6—C7109.7
C1—N1—C1v111.81 (8)H6B—C6—C7109.7
N1—C1—H1A108.0C6—C7—H7A108.8
N1—C1—H1B108.0C6—C7—H7B108.8
N1—C1—C2117.25 (14)C6—C7—C8113.7 (2)
H1A—C1—H1B107.2H7A—C7—H7B107.7
H1A—C1—C2108.0H7A—C7—C8108.8
H1B—C1—C2108.0H7B—C7—C8108.8
C1—C2—H2A110.1C7—C8—H8A109.5
C1—C2—H2B110.1C7—C8—H8B109.5
C1—C2—C3108.14 (17)C7—C8—H8C109.5
H2A—C2—H2B108.4H8A—C8—H8B109.5
H2A—C2—C3110.1H8A—C8—H8C109.5
H2B—C2—C3110.1H8B—C8—H8C109.5
C1iv—N1—C1—C2175.0 (2)C5vii—N2—C5—C661.8 (2)
C1vi—N1—C1—C263.7 (2)C5viii—N2—C5—C655.6 (2)
C1v—N1—C1—C253.6 (2)C5iv—N2—C5—C6176.9 (2)
N1—C1—C2—C3174.11 (15)N2—C5—C6—C7173.47 (16)
C1—C2—C3—C4172.65 (19)C5—C6—C7—C874.8 (3)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) y+1/2, x, z; (iii) y, x+1/2, z; (iv) x+3/2, y+1/2, z; (v) y+1/2, x+1, z; (vi) y+1, x1/2, z; (vii) y+1/2, x+1, z+1; (viii) y+1, x1/2, z+1.
 

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