metal-organic compounds
The title complex, (C8H20N)2[MoS4(CuCN)2]·H2O, contains an anion in which Cu atoms bridge two opposite SS 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
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201070X/bt6150sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680201070X/bt6150Isup2.hkl |
CCDC reference: 168475
Key indicators
- Single-crystal X-ray study
- T = 160 K
- Mean (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
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]·H2O | F(000) = 1400 |
Mr = 681.82 | Dx = 1.539 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 14.1202 (5) Å | Cell parameters from 19634 reflections |
b = 7.1989 (3) Å | θ = 2.3–28.6° |
c = 29.3581 (10) Å | µ = 2.15 mm−1 |
β = 99.592 (2)° | T = 160 K |
V = 2942.53 (19) Å3 | Block, orange |
Z = 4 | 0.36 × 0.26 × 0.16 mm |
Data collection top
Bruker SMART CCD diffractometer | 7028 independent reflections |
Radiation source: fine-focus sealed tube | 6142 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 8.192 pixels mm-1 | θmax = 28.6°, θmin = 1.7° |
ω rotation with narrow frames scans | h = −18→18 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1997a) | k = −9→9 |
Tmin = 0.511, Tmax = 0.725 | l = −38→39 |
24398 measured reflections |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.024 | H 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 reflections | Δρmax = 0.42 e Å−3 |
288 parameters | Δρmin = −0.36 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00051 (8) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Mo | 0.778068 (10) | 0.73485 (2) | 0.613186 (5) | 0.02367 (5) | |
S1 | 0.87452 (3) | 0.73525 (7) | 0.560607 (16) | 0.02997 (10) | |
S2 | 0.85343 (4) | 0.88526 (7) | 0.674149 (17) | 0.03474 (11) | |
S3 | 0.74611 (3) | 0.44865 (7) | 0.633126 (16) | 0.03043 (10) | |
S4 | 0.63931 (4) | 0.87262 (7) | 0.587334 (19) | 0.03657 (12) | |
Cu1 | 0.949058 (16) | 0.88778 (3) | 0.621687 (8) | 0.02974 (6) | |
C1 | 1.07246 (14) | 0.9966 (3) | 0.62972 (7) | 0.0336 (4) | |
N1 | 1.14702 (13) | 1.0610 (3) | 0.63486 (7) | 0.0478 (5) | |
Cu2 | 0.607099 (16) | 0.59106 (3) | 0.610582 (8) | 0.03120 (6) | |
C2 | 0.48418 (14) | 0.5023 (3) | 0.61730 (7) | 0.0324 (4) | |
N2 | 0.41147 (12) | 0.4554 (3) | 0.62476 (7) | 0.0432 (4) | |
N3 | 1.00752 (11) | 0.3916 (2) | 0.75999 (5) | 0.0264 (3) | |
C3 | 0.90851 (14) | 0.3327 (3) | 0.73621 (7) | 0.0364 (4) | |
H3A | 0.8693 | 0.4457 | 0.7280 | 0.044* | |
H3B | 0.9150 | 0.2688 | 0.7070 | 0.044* | |
C4 | 0.85506 (17) | 0.2060 (4) | 0.76431 (8) | 0.0491 (6) | |
H4A | 0.8925 | 0.0925 | 0.7722 | 0.074* | |
H4B | 0.7925 | 0.1739 | 0.7462 | 0.074* | |
H4C | 0.8456 | 0.2697 | 0.7927 | 0.074* | |
C5 | 1.00345 (14) | 0.4711 (3) | 0.80763 (6) | 0.0310 (4) | |
H5A | 0.9900 | 0.3684 | 0.8281 | 0.037* | |
H5B | 1.0675 | 0.5218 | 0.8205 | 0.037* | |
C6 | 0.92986 (17) | 0.6212 (3) | 0.80906 (8) | 0.0445 (5) | |
H6A | 0.9439 | 0.7264 | 0.7901 | 0.067* | |
H6B | 0.9320 | 0.6625 | 0.8410 | 0.067* | |
H6C | 0.8658 | 0.5725 | 0.7970 | 0.067* | |
C7 | 1.04516 (15) | 0.5426 (3) | 0.73140 (7) | 0.0333 (4) | |
H7A | 0.9995 | 0.6480 | 0.7283 | 0.040* | |
H7B | 1.1072 | 0.5880 | 0.7485 | 0.040* | |
C8 | 1.05984 (17) | 0.4838 (3) | 0.68367 (7) | 0.0450 (5) | |
H8A | 1.1053 | 0.3800 | 0.6862 | 0.068* | |
H8B | 1.0855 | 0.5885 | 0.6682 | 0.068* | |
H8C | 0.9983 | 0.4449 | 0.6657 | 0.068* | |
C9 | 1.07298 (15) | 0.2228 (3) | 0.76485 (7) | 0.0366 (4) | |
H9A | 1.0486 | 0.1324 | 0.7855 | 0.044* | |
H9B | 1.0687 | 0.1636 | 0.7341 | 0.044* | |
C10 | 1.17764 (16) | 0.2603 (3) | 0.78349 (9) | 0.0510 (6) | |
H10A | 1.2048 | 0.3399 | 0.7618 | 0.077* | |
H10B | 1.2129 | 0.1425 | 0.7873 | 0.077* | |
H10C | 1.1831 | 0.3229 | 0.8135 | 0.077* | |
N4 | 0.76295 (11) | 0.2435 (2) | 0.47284 (5) | 0.0271 (3) | |
C11 | 0.85946 (15) | 0.1487 (3) | 0.48631 (7) | 0.0348 (4) | |
H11A | 0.8890 | 0.1339 | 0.4582 | 0.042* | |
H11B | 0.8484 | 0.0228 | 0.4979 | 0.042* | |
C12 | 0.93053 (16) | 0.2489 (3) | 0.52267 (8) | 0.0428 (5) | |
H12A | 0.9441 | 0.3723 | 0.5112 | 0.064* | |
H12B | 0.9903 | 0.1772 | 0.5292 | 0.064* | |
H12C | 0.9031 | 0.2617 | 0.5510 | 0.064* | |
C13 | 0.77522 (14) | 0.4405 (2) | 0.45617 (6) | 0.0295 (4) | |
H13A | 0.7108 | 0.4943 | 0.4456 | 0.035* | |
H13B | 0.8066 | 0.5158 | 0.4827 | 0.035* | |
C14 | 0.83351 (16) | 0.4574 (3) | 0.41737 (7) | 0.0407 (5) | |
H14A | 0.8981 | 0.4073 | 0.4276 | 0.061* | |
H14B | 0.8382 | 0.5884 | 0.4090 | 0.061* | |
H14C | 0.8019 | 0.3872 | 0.3905 | 0.061* | |
C15 | 0.70351 (15) | 0.1337 (3) | 0.43394 (7) | 0.0341 (4) | |
H15A | 0.6448 | 0.2055 | 0.4220 | 0.041* | |
H15B | 0.7409 | 0.1212 | 0.4084 | 0.041* | |
C16 | 0.6740 (2) | −0.0585 (3) | 0.44732 (9) | 0.0577 (7) | |
H16A | 0.7314 | −0.1306 | 0.4597 | 0.087* | |
H16B | 0.6389 | −0.1215 | 0.4200 | 0.087* | |
H16C | 0.6326 | −0.0478 | 0.4709 | 0.087* | |
C17 | 0.71310 (15) | 0.2522 (3) | 0.51470 (7) | 0.0368 (5) | |
H17A | 0.7123 | 0.1258 | 0.5279 | 0.044* | |
H17B | 0.7516 | 0.3321 | 0.5383 | 0.044* | |
C18 | 0.61144 (16) | 0.3252 (4) | 0.50570 (8) | 0.0515 (6) | |
H18A | 0.6114 | 0.4530 | 0.4942 | 0.077* | |
H18B | 0.5849 | 0.3231 | 0.5345 | 0.077* | |
H18C | 0.5721 | 0.2469 | 0.4826 | 0.077* | |
O1 | 0.30345 (13) | 0.2693 (3) | 0.68701 (6) | 0.0472 (4) | |
H1A | 0.261 (2) | 0.214 (4) | 0.6721 (11) | 0.068 (10)* | |
H1B | 0.3263 (19) | 0.324 (4) | 0.6682 (10) | 0.055 (9)* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo | 0.02510 (8) | 0.02423 (8) | 0.02190 (8) | −0.00257 (6) | 0.00457 (6) | −0.00003 (6) |
S1 | 0.0342 (2) | 0.0325 (2) | 0.0245 (2) | −0.00403 (18) | 0.00871 (18) | −0.00215 (18) |
S2 | 0.0377 (3) | 0.0391 (3) | 0.0288 (2) | −0.0091 (2) | 0.00953 (19) | −0.0104 (2) |
S3 | 0.0326 (2) | 0.0284 (2) | 0.0292 (2) | −0.00338 (18) | 0.00193 (18) | 0.00410 (18) |
S4 | 0.0306 (2) | 0.0352 (3) | 0.0444 (3) | 0.0023 (2) | 0.0075 (2) | 0.0112 (2) |
Cu1 | 0.02803 (12) | 0.03011 (12) | 0.03154 (12) | −0.00591 (9) | 0.00631 (9) | −0.00216 (9) |
C1 | 0.0358 (10) | 0.0308 (10) | 0.0352 (10) | −0.0041 (8) | 0.0086 (8) | −0.0047 (8) |
N1 | 0.0373 (10) | 0.0452 (11) | 0.0625 (13) | −0.0099 (8) | 0.0132 (9) | −0.0114 (9) |
Cu2 | 0.02688 (12) | 0.03591 (13) | 0.03048 (12) | −0.00653 (9) | 0.00378 (9) | 0.00275 (10) |
C2 | 0.0298 (10) | 0.0321 (10) | 0.0329 (10) | −0.0018 (8) | −0.0018 (8) | 0.0035 (8) |
N2 | 0.0303 (9) | 0.0499 (11) | 0.0476 (11) | −0.0082 (8) | 0.0012 (8) | 0.0063 (9) |
N3 | 0.0301 (8) | 0.0269 (8) | 0.0224 (7) | 0.0028 (6) | 0.0047 (6) | 0.0005 (6) |
C3 | 0.0348 (10) | 0.0433 (11) | 0.0293 (10) | −0.0022 (9) | 0.0001 (8) | −0.0106 (9) |
C4 | 0.0436 (13) | 0.0595 (15) | 0.0472 (13) | −0.0189 (11) | 0.0157 (10) | −0.0203 (11) |
C5 | 0.0359 (10) | 0.0341 (10) | 0.0226 (9) | −0.0041 (8) | 0.0033 (7) | −0.0039 (7) |
C6 | 0.0558 (14) | 0.0389 (12) | 0.0402 (12) | 0.0032 (10) | 0.0124 (10) | −0.0119 (10) |
C7 | 0.0388 (10) | 0.0314 (10) | 0.0304 (10) | 0.0026 (8) | 0.0078 (8) | 0.0076 (8) |
C8 | 0.0548 (14) | 0.0500 (13) | 0.0339 (11) | 0.0128 (11) | 0.0181 (10) | 0.0100 (10) |
C9 | 0.0424 (11) | 0.0301 (10) | 0.0390 (11) | 0.0089 (8) | 0.0117 (9) | 0.0048 (8) |
C10 | 0.0402 (12) | 0.0581 (15) | 0.0547 (14) | 0.0159 (11) | 0.0077 (10) | 0.0165 (12) |
N4 | 0.0377 (8) | 0.0210 (7) | 0.0232 (7) | 0.0007 (6) | 0.0063 (6) | −0.0001 (6) |
C11 | 0.0438 (11) | 0.0268 (9) | 0.0329 (10) | 0.0092 (8) | 0.0041 (8) | 0.0048 (8) |
C12 | 0.0417 (12) | 0.0412 (12) | 0.0428 (12) | 0.0071 (9) | −0.0015 (9) | 0.0027 (10) |
C13 | 0.0387 (10) | 0.0200 (8) | 0.0285 (9) | 0.0016 (7) | 0.0018 (7) | 0.0017 (7) |
C14 | 0.0446 (12) | 0.0387 (11) | 0.0396 (11) | −0.0013 (9) | 0.0097 (9) | 0.0111 (9) |
C15 | 0.0456 (11) | 0.0295 (10) | 0.0262 (9) | −0.0038 (8) | 0.0035 (8) | −0.0052 (8) |
C16 | 0.0806 (19) | 0.0335 (12) | 0.0558 (15) | −0.0192 (12) | 0.0021 (13) | −0.0040 (11) |
C17 | 0.0461 (12) | 0.0417 (12) | 0.0243 (9) | −0.0022 (9) | 0.0106 (8) | −0.0004 (8) |
C18 | 0.0439 (13) | 0.0741 (17) | 0.0394 (12) | 0.0020 (12) | 0.0152 (10) | −0.0079 (12) |
O1 | 0.0376 (9) | 0.0564 (11) | 0.0457 (10) | −0.0091 (8) | 0.0019 (8) | 0.0081 (8) |
Geometric parameters (Å, º) top
Mo—S1 | 2.2222 (5) | N3—C7 | 1.522 (2) |
Mo—S2 | 2.2076 (5) | N3—C9 | 1.519 (2) |
Mo—S3 | 2.2089 (5) | C3—C4 | 1.513 (3) |
Mo—S4 | 2.2143 (5) | C5—C6 | 1.505 (3) |
S1—Cu1 | 2.2136 (5) | C7—C8 | 1.510 (3) |
S2—Cu1 | 2.2111 (5) | C9—C10 | 1.512 (3) |
S3—Cu2 | 2.2156 (5) | N4—C11 | 1.516 (2) |
S4—Cu2 | 2.2101 (5) | N4—C13 | 1.520 (2) |
Cu1—C1 | 1.889 (2) | N4—C15 | 1.521 (2) |
C1—N1 | 1.137 (3) | N4—C17 | 1.516 (2) |
Cu2—C2 | 1.890 (2) | C11—C12 | 1.520 (3) |
C2—N2 | 1.136 (3) | C13—C14 | 1.517 (3) |
N3—C3 | 1.515 (2) | C15—C16 | 1.516 (3) |
N3—C5 | 1.521 (2) | C17—C18 | 1.510 (3) |
S1—Mo—S2 | 107.103 (19) | C3—N3—C7 | 109.01 (15) |
S1—Mo—S3 | 111.174 (19) | C3—N3—C9 | 108.66 (15) |
S1—Mo—S4 | 111.78 (2) | C5—N3—C7 | 107.97 (14) |
S2—Mo—S3 | 109.561 (19) | C5—N3—C9 | 109.29 (14) |
S2—Mo—S4 | 109.73 (2) | C7—N3—C9 | 111.10 (15) |
S3—Mo—S4 | 107.483 (19) | N3—C3—C4 | 115.03 (17) |
Mo—S1—Cu1 | 72.640 (15) | N3—C5—C6 | 115.34 (16) |
Mo—S2—Cu1 | 72.968 (16) | N3—C7—C8 | 115.23 (17) |
Mo—S3—Cu2 | 72.494 (16) | N3—C9—C10 | 115.71 (17) |
Mo—S4—Cu2 | 72.496 (17) | C11—N4—C13 | 111.00 (15) |
S1—Cu1—S2 | 107.285 (19) | C11—N4—C15 | 108.74 (14) |
S1—Cu1—C1 | 127.66 (6) | C11—N4—C17 | 109.01 (14) |
S2—Cu1—C1 | 125.04 (6) | C13—N4—C15 | 108.75 (14) |
Cu1—C1—N1 | 179.4 (2) | C13—N4—C17 | 108.39 (14) |
S3—Cu2—S4 | 107.40 (2) | C15—N4—C17 | 110.95 (15) |
S3—Cu2—C2 | 126.55 (6) | N4—C11—C12 | 115.41 (16) |
S4—Cu2—C2 | 125.59 (6) | N4—C13—C14 | 114.93 (15) |
Cu2—C2—N2 | 174.46 (19) | N4—C15—C16 | 114.89 (17) |
C3—N3—C5 | 110.82 (14) | N4—C17—C18 | 115.39 (17) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···N1i | 0.79 (3) | 2.10 (3) | 2.889 (3) | 178 (3) |
O1—H1B···N2 | 0.79 (3) | 2.12 (3) | 2.897 (3) | 170 (3) |
Symmetry code: (i) x−1, y−1, z. |