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The title complex, (C8H20N)2[MoS4(CuCN)2]·H2O, contains an anion in which Cu atoms bridge two opposite S...S edges of the central MoS4 unit. The Mo atom retains tetrahedral coordination geometry, while each Cu is trigonal planar coordinated by two bridging sulfides and a terminal cyano ligand. The anions are linked together into chains by hydrogen bonding to ordered water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201070X/bt6150sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680201070X/bt6150Isup2.hkl
Contains datablock I

CCDC reference: 168475

Key indicators

  • Single-crystal X-ray study
  • T = 160 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.024
  • wR factor = 0.056
  • Data-to-parameter ratio = 24.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 28.60 From the CIF: _reflns_number_total 7028 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 7532 Completeness (_total/calc) 93.31% Alert C: < 95% complete
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997b); 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
(C8H20N)2[Cu2MoS4(CN)2]·H2OF(000) = 1400
Mr = 681.82Dx = 1.539 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 14.1202 (5) ÅCell parameters from 19634 reflections
b = 7.1989 (3) Åθ = 2.3–28.6°
c = 29.3581 (10) ŵ = 2.15 mm1
β = 99.592 (2)°T = 160 K
V = 2942.53 (19) Å3Block, orange
Z = 40.36 × 0.26 × 0.16 mm
Data collection top
Bruker SMART CCD
diffractometer
7028 independent reflections
Radiation source: fine-focus sealed tube6142 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Detector resolution: 8.192 pixels mm-1θmax = 28.6°, θmin = 1.7°
ω rotation with narrow frames scansh = 1818
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997a)
k = 99
Tmin = 0.511, Tmax = 0.725l = 3839
24398 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.056 w = 1/[σ2(Fo2) + (0.0244P)2 + 1.151P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.003
7028 reflectionsΔρmax = 0.42 e Å3
288 parametersΔρmin = 0.36 e Å3
0 restraintsExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00051 (8)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo0.778068 (10)0.73485 (2)0.613186 (5)0.02367 (5)
S10.87452 (3)0.73525 (7)0.560607 (16)0.02997 (10)
S20.85343 (4)0.88526 (7)0.674149 (17)0.03474 (11)
S30.74611 (3)0.44865 (7)0.633126 (16)0.03043 (10)
S40.63931 (4)0.87262 (7)0.587334 (19)0.03657 (12)
Cu10.949058 (16)0.88778 (3)0.621687 (8)0.02974 (6)
C11.07246 (14)0.9966 (3)0.62972 (7)0.0336 (4)
N11.14702 (13)1.0610 (3)0.63486 (7)0.0478 (5)
Cu20.607099 (16)0.59106 (3)0.610582 (8)0.03120 (6)
C20.48418 (14)0.5023 (3)0.61730 (7)0.0324 (4)
N20.41147 (12)0.4554 (3)0.62476 (7)0.0432 (4)
N31.00752 (11)0.3916 (2)0.75999 (5)0.0264 (3)
C30.90851 (14)0.3327 (3)0.73621 (7)0.0364 (4)
H3A0.86930.44570.72800.044*
H3B0.91500.26880.70700.044*
C40.85506 (17)0.2060 (4)0.76431 (8)0.0491 (6)
H4A0.89250.09250.77220.074*
H4B0.79250.17390.74620.074*
H4C0.84560.26970.79270.074*
C51.00345 (14)0.4711 (3)0.80763 (6)0.0310 (4)
H5A0.99000.36840.82810.037*
H5B1.06750.52180.82050.037*
C60.92986 (17)0.6212 (3)0.80906 (8)0.0445 (5)
H6A0.94390.72640.79010.067*
H6B0.93200.66250.84100.067*
H6C0.86580.57250.79700.067*
C71.04516 (15)0.5426 (3)0.73140 (7)0.0333 (4)
H7A0.99950.64800.72830.040*
H7B1.10720.58800.74850.040*
C81.05984 (17)0.4838 (3)0.68367 (7)0.0450 (5)
H8A1.10530.38000.68620.068*
H8B1.08550.58850.66820.068*
H8C0.99830.44490.66570.068*
C91.07298 (15)0.2228 (3)0.76485 (7)0.0366 (4)
H9A1.04860.13240.78550.044*
H9B1.06870.16360.73410.044*
C101.17764 (16)0.2603 (3)0.78349 (9)0.0510 (6)
H10A1.20480.33990.76180.077*
H10B1.21290.14250.78730.077*
H10C1.18310.32290.81350.077*
N40.76295 (11)0.2435 (2)0.47284 (5)0.0271 (3)
C110.85946 (15)0.1487 (3)0.48631 (7)0.0348 (4)
H11A0.88900.13390.45820.042*
H11B0.84840.02280.49790.042*
C120.93053 (16)0.2489 (3)0.52267 (8)0.0428 (5)
H12A0.94410.37230.51120.064*
H12B0.99030.17720.52920.064*
H12C0.90310.26170.55100.064*
C130.77522 (14)0.4405 (2)0.45617 (6)0.0295 (4)
H13A0.71080.49430.44560.035*
H13B0.80660.51580.48270.035*
C140.83351 (16)0.4574 (3)0.41737 (7)0.0407 (5)
H14A0.89810.40730.42760.061*
H14B0.83820.58840.40900.061*
H14C0.80190.38720.39050.061*
C150.70351 (15)0.1337 (3)0.43394 (7)0.0341 (4)
H15A0.64480.20550.42200.041*
H15B0.74090.12120.40840.041*
C160.6740 (2)0.0585 (3)0.44732 (9)0.0577 (7)
H16A0.73140.13060.45970.087*
H16B0.63890.12150.42000.087*
H16C0.63260.04780.47090.087*
C170.71310 (15)0.2522 (3)0.51470 (7)0.0368 (5)
H17A0.71230.12580.52790.044*
H17B0.75160.33210.53830.044*
C180.61144 (16)0.3252 (4)0.50570 (8)0.0515 (6)
H18A0.61140.45300.49420.077*
H18B0.58490.32310.53450.077*
H18C0.57210.24690.48260.077*
O10.30345 (13)0.2693 (3)0.68701 (6)0.0472 (4)
H1A0.261 (2)0.214 (4)0.6721 (11)0.068 (10)*
H1B0.3263 (19)0.324 (4)0.6682 (10)0.055 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo0.02510 (8)0.02423 (8)0.02190 (8)0.00257 (6)0.00457 (6)0.00003 (6)
S10.0342 (2)0.0325 (2)0.0245 (2)0.00403 (18)0.00871 (18)0.00215 (18)
S20.0377 (3)0.0391 (3)0.0288 (2)0.0091 (2)0.00953 (19)0.0104 (2)
S30.0326 (2)0.0284 (2)0.0292 (2)0.00338 (18)0.00193 (18)0.00410 (18)
S40.0306 (2)0.0352 (3)0.0444 (3)0.0023 (2)0.0075 (2)0.0112 (2)
Cu10.02803 (12)0.03011 (12)0.03154 (12)0.00591 (9)0.00631 (9)0.00216 (9)
C10.0358 (10)0.0308 (10)0.0352 (10)0.0041 (8)0.0086 (8)0.0047 (8)
N10.0373 (10)0.0452 (11)0.0625 (13)0.0099 (8)0.0132 (9)0.0114 (9)
Cu20.02688 (12)0.03591 (13)0.03048 (12)0.00653 (9)0.00378 (9)0.00275 (10)
C20.0298 (10)0.0321 (10)0.0329 (10)0.0018 (8)0.0018 (8)0.0035 (8)
N20.0303 (9)0.0499 (11)0.0476 (11)0.0082 (8)0.0012 (8)0.0063 (9)
N30.0301 (8)0.0269 (8)0.0224 (7)0.0028 (6)0.0047 (6)0.0005 (6)
C30.0348 (10)0.0433 (11)0.0293 (10)0.0022 (9)0.0001 (8)0.0106 (9)
C40.0436 (13)0.0595 (15)0.0472 (13)0.0189 (11)0.0157 (10)0.0203 (11)
C50.0359 (10)0.0341 (10)0.0226 (9)0.0041 (8)0.0033 (7)0.0039 (7)
C60.0558 (14)0.0389 (12)0.0402 (12)0.0032 (10)0.0124 (10)0.0119 (10)
C70.0388 (10)0.0314 (10)0.0304 (10)0.0026 (8)0.0078 (8)0.0076 (8)
C80.0548 (14)0.0500 (13)0.0339 (11)0.0128 (11)0.0181 (10)0.0100 (10)
C90.0424 (11)0.0301 (10)0.0390 (11)0.0089 (8)0.0117 (9)0.0048 (8)
C100.0402 (12)0.0581 (15)0.0547 (14)0.0159 (11)0.0077 (10)0.0165 (12)
N40.0377 (8)0.0210 (7)0.0232 (7)0.0007 (6)0.0063 (6)0.0001 (6)
C110.0438 (11)0.0268 (9)0.0329 (10)0.0092 (8)0.0041 (8)0.0048 (8)
C120.0417 (12)0.0412 (12)0.0428 (12)0.0071 (9)0.0015 (9)0.0027 (10)
C130.0387 (10)0.0200 (8)0.0285 (9)0.0016 (7)0.0018 (7)0.0017 (7)
C140.0446 (12)0.0387 (11)0.0396 (11)0.0013 (9)0.0097 (9)0.0111 (9)
C150.0456 (11)0.0295 (10)0.0262 (9)0.0038 (8)0.0035 (8)0.0052 (8)
C160.0806 (19)0.0335 (12)0.0558 (15)0.0192 (12)0.0021 (13)0.0040 (11)
C170.0461 (12)0.0417 (12)0.0243 (9)0.0022 (9)0.0106 (8)0.0004 (8)
C180.0439 (13)0.0741 (17)0.0394 (12)0.0020 (12)0.0152 (10)0.0079 (12)
O10.0376 (9)0.0564 (11)0.0457 (10)0.0091 (8)0.0019 (8)0.0081 (8)
Geometric parameters (Å, º) top
Mo—S12.2222 (5)N3—C71.522 (2)
Mo—S22.2076 (5)N3—C91.519 (2)
Mo—S32.2089 (5)C3—C41.513 (3)
Mo—S42.2143 (5)C5—C61.505 (3)
S1—Cu12.2136 (5)C7—C81.510 (3)
S2—Cu12.2111 (5)C9—C101.512 (3)
S3—Cu22.2156 (5)N4—C111.516 (2)
S4—Cu22.2101 (5)N4—C131.520 (2)
Cu1—C11.889 (2)N4—C151.521 (2)
C1—N11.137 (3)N4—C171.516 (2)
Cu2—C21.890 (2)C11—C121.520 (3)
C2—N21.136 (3)C13—C141.517 (3)
N3—C31.515 (2)C15—C161.516 (3)
N3—C51.521 (2)C17—C181.510 (3)
S1—Mo—S2107.103 (19)C3—N3—C7109.01 (15)
S1—Mo—S3111.174 (19)C3—N3—C9108.66 (15)
S1—Mo—S4111.78 (2)C5—N3—C7107.97 (14)
S2—Mo—S3109.561 (19)C5—N3—C9109.29 (14)
S2—Mo—S4109.73 (2)C7—N3—C9111.10 (15)
S3—Mo—S4107.483 (19)N3—C3—C4115.03 (17)
Mo—S1—Cu172.640 (15)N3—C5—C6115.34 (16)
Mo—S2—Cu172.968 (16)N3—C7—C8115.23 (17)
Mo—S3—Cu272.494 (16)N3—C9—C10115.71 (17)
Mo—S4—Cu272.496 (17)C11—N4—C13111.00 (15)
S1—Cu1—S2107.285 (19)C11—N4—C15108.74 (14)
S1—Cu1—C1127.66 (6)C11—N4—C17109.01 (14)
S2—Cu1—C1125.04 (6)C13—N4—C15108.75 (14)
Cu1—C1—N1179.4 (2)C13—N4—C17108.39 (14)
S3—Cu2—S4107.40 (2)C15—N4—C17110.95 (15)
S3—Cu2—C2126.55 (6)N4—C11—C12115.41 (16)
S4—Cu2—C2125.59 (6)N4—C13—C14114.93 (15)
Cu2—C2—N2174.46 (19)N4—C15—C16114.89 (17)
C3—N3—C5110.82 (14)N4—C17—C18115.39 (17)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···N1i0.79 (3)2.10 (3)2.889 (3)178 (3)
O1—H1B···N20.79 (3)2.12 (3)2.897 (3)170 (3)
Symmetry code: (i) x1, y1, z.
 

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