The Cu atom in the title compound, [Cu(C7H6NO2S)2(H2O)2(NH3)2], lies on a special position at a crystallographic inversion centre and has a tetragonally distorted octahedral coordination involving the N atoms of two ammine ligands [Cu-N = 2.010 (2) Å], the N atoms of two pyridylthioacetate ligands [Cu-N = 2.033 (2) Å] and the O atoms of two water molecules [Cu-O = 2.472 (2) Å].
Supporting information
CCDC reference: 234783
Key indicators
- Single-crystal X-ray study
- T = 298 K
- R factor = 0.034
- wR factor = 0.090
- Data-to-parameter ratio = 14.9
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.434 0.841
Tmin' and Tmax expected: 0.555 0.841
RR' = 0.783
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.76
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - O1W = 7.09 su
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.06
PLAT706_ALERT_1_C H...A Calc 2.143(15), Rep 2.160(10), Dev.. 1.13 Sigma
H3# -O1 1.555 2.554
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 5
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 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
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Diamminediaquabis(4-pyridylthioacetato)copper(II)
top
Crystal data top
[Cu(C7H6NO2S)2(H2O)2(NH3)2] | F(000) = 972 |
Mr = 470.02 | Dx = 1.677 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 23.263 (1) Å | Cell parameters from 6563 reflections |
b = 7.0762 (3) Å | θ = 3.0–28.3° |
c = 11.5216 (5) Å | µ = 1.44 mm−1 |
β = 100.989 (1)° | T = 298 K |
V = 1861.8 (1) Å3 | Plate, blue |
Z = 4 | 0.40 × 0.30 × 0.12 mm |
Data collection top
Bruker APEX area-detector diffractometer | 2139 independent reflections |
Radiation source: fine-focus sealed tube | 1744 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
φ and ω scan | θmax = 27.5°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −30→30 |
Tmin = 0.434, Tmax = 0.841 | k = −9→9 |
10239 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.090 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0477P)2] where P = (Fo2 + 2Fc2)/3 |
2139 reflections | (Δ/σ)max = 0.001 |
144 parameters | Δρmax = 0.40 e Å−3 |
5 restraints | Δρmin = −0.48 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.2500 | 0.2500 | 0.0000 | 0.0228 (1) | |
S1 | −0.02126 (2) | 0.26497 (8) | 0.08209 (5) | 0.0344 (2) | |
O1 | −0.17033 (7) | 0.2496 (2) | −0.1354 (2) | 0.0403 (4) | |
O2 | −0.14202 (7) | 0.2702 (2) | 0.0598 (2) | 0.0398 (4) | |
O1w | 0.2699 (1) | 0.5376 (2) | 0.1228 (1) | 0.0356 (4) | |
N1 | 0.1649 (1) | 0.2402 (2) | 0.0191 (2) | 0.0252 (4) | |
N2 | 0.2269 (1) | 0.4358 (3) | −0.1326 (2) | 0.0280 (4) | |
C1 | 0.1515 (1) | 0.2612 (2) | 0.1263 (2) | 0.0273 (4) | |
C2 | 0.0951 (1) | 0.2676 (2) | 0.1459 (2) | 0.0285 (5) | |
C3 | 0.0489 (1) | 0.2527 (2) | 0.0496 (2) | 0.0256 (4) | |
C4 | 0.0624 (1) | 0.2284 (3) | −0.0617 (2) | 0.0302 (5) | |
C5 | 0.1202 (1) | 0.2222 (3) | −0.0726 (2) | 0.0295 (5) | |
C6 | −0.0693 (1) | 0.2479 (2) | −0.0592 (2) | 0.0279 (5) | |
C7 | −0.1330 (1) | 0.2574 (2) | −0.0429 (2) | 0.0295 (5) | |
H2n1 | 0.202 (1) | 0.522 (2) | −0.113 (2) | 0.028 (6)* | |
H2n2 | 0.257 (1) | 0.507 (3) | −0.141 (2) | 0.070 (9)* | |
H2n3 | 0.209 (1) | 0.379 (3) | −0.200 (1) | 0.055 (8)* | |
H1w1 | 0.242 (1) | 0.612 (3) | 0.115 (2) | 0.036 (6)* | |
H1w2 | 0.296 (1) | 0.601 (3) | 0.102 (2) | 0.039 (7)* | |
H1 | 0.1820 | 0.2722 | 0.1911 | 0.033* | |
H2 | 0.0879 | 0.2816 | 0.2221 | 0.034* | |
H4 | 0.0328 | 0.2166 | −0.1280 | 0.036* | |
H5 | 0.1288 | 0.2046 | −0.1475 | 0.035* | |
H6a | −0.0614 | 0.3506 | −0.1097 | 0.033* | |
H6b | −0.0625 | 0.1296 | −0.0969 | 0.033* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0139 (2) | 0.0331 (2) | 0.0213 (2) | 0.0020 (1) | 0.0030 (1) | 0.0040 (1) |
S1 | 0.0159 (3) | 0.0559 (4) | 0.0317 (3) | 0.0003 (2) | 0.0056 (2) | −0.0022 (2) |
O1 | 0.021 (1) | 0.058 (1) | 0.039 (1) | 0.001 (1) | −0.001 (1) | 0.002 (1) |
O2 | 0.023 (1) | 0.060 (1) | 0.037 (1) | 0.001 (1) | 0.008 (1) | −0.002 (1) |
N1 | 0.017 (1) | 0.033 (1) | 0.026 (1) | 0.002 (1) | 0.003 (1) | 0.001 (1) |
N2 | 0.023 (1) | 0.036 (1) | 0.024 (1) | 0.003 (1) | 0.003 (1) | 0.003 (1) |
O1w | 0.026 (1) | 0.045 (1) | 0.038 (1) | 0.000 (1) | 0.009 (1) | −0.003 (1) |
C1 | 0.020 (1) | 0.037 (1) | 0.024 (1) | 0.000 (1) | 0.001 (1) | −0.001 (1) |
C2 | 0.021 (1) | 0.038 (1) | 0.027 (1) | 0.001 (1) | 0.006 (1) | −0.001 (1) |
C3 | 0.018 (1) | 0.028 (1) | 0.032 (1) | 0.000 (1) | 0.006 (1) | 0.001 (1) |
C4 | 0.019 (1) | 0.043 (1) | 0.027 (1) | −0.001 (1) | 0.000 (1) | −0.002 (1) |
C5 | 0.022 (1) | 0.042 (1) | 0.024 (1) | 0.001 (1) | 0.003 (1) | −0.001 (1) |
C6 | 0.019 (1) | 0.033 (1) | 0.031 (1) | 0.001 (1) | 0.005 (1) | 0.000 (1) |
C7 | 0.019 (1) | 0.027 (1) | 0.042 (1) | 0.002 (1) | 0.006 (1) | 0.003 (1) |
Geometric parameters (Å, º) top
Cu1—N1 | 2.033 (2) | C3—C4 | 1.388 (3) |
Cu1—N1i | 2.033 (2) | C4—C5 | 1.375 (3) |
Cu1—N2 | 2.010 (2) | C6—C7 | 1.530 (3) |
Cu1—N2i | 2.010 (2) | N2—H2n1 | 0.89 (1) |
Cu1—O1w | 2.472 (2) | N2—H2n2 | 0.88 (1) |
Cu1—O1wi | 2.472 (2) | N2—H2n3 | 0.89 (1) |
S1—C3 | 1.745 (2) | O1w—H1w1 | 0.83 (1) |
S1—C6 | 1.795 (2) | O1w—H1w2 | 0.82 (1) |
O1—C7 | 1.242 (3) | C1—H1 | 0.93 |
O2—C7 | 1.245 (3) | C2—H2 | 0.93 |
N1—C5 | 1.340 (3) | C4—H4 | 0.93 |
N1—C1 | 1.339 (3) | C5—H5 | 0.93 |
C1—C2 | 1.373 (3) | C6—H6a | 0.97 |
C2—C3 | 1.394 (3) | C6—H6b | 0.97 |
| | | |
N1—Cu1—N1i | 180 | C7—C6—S1 | 109.6 (2) |
N1—Cu1—N2 | 88.9 (1) | O1—C7—O2 | 127.0 (2) |
N1—Cu1—N2i | 91.1 (1) | O1—C7—C6 | 115.4 (2) |
N1—Cu1—O1w | 92.7 (1) | O2—C7—C6 | 117.6 (2) |
N1—Cu1—O1wi | 87.3 (1) | Cu1—N2—H2n1 | 110 (1) |
N1i—Cu1—N2 | 91.1 (1) | Cu1—N2—H2n2 | 111 (2) |
N1i—Cu1—N2i | 88.9 (1) | H2n1—N2—H2n2 | 101 (2) |
N1i—Cu1—O1w | 87.3 (1) | Cu1—N2—H2n3 | 112 (2) |
N1i—Cu1—O1wi | 92.7 (1) | H2n1—N2—H2n3 | 108 (2) |
N2—Cu1—N2i | 180 | H2n2—N2—H2n3 | 114 (2) |
N2—Cu1—O1w | 83.7 (1) | Cu1—O1w—H1w1 | 114 (2) |
N2—Cu1—O1wi | 96.3 (1) | Cu1—O1w—H1w2 | 110 (2) |
N2i—Cu1—O1w | 96.3 (1) | H1w1—O1w—H1w2 | 103 (2) |
N2i—Cu1—O1wi | 83.7 (1) | N1—C1—H1 | 118.2 |
O1w—Cu1—O1wi | 180 | C2—C1—H1 | 118.2 |
C3—S1—C6 | 104.3 (1) | C1—C2—H2 | 120.6 |
C5—N1—C1 | 117.1 (2) | C3—C2—H2 | 120.6 |
C5—N1—Cu1 | 122.9 (2) | C5—C4—H4 | 120.5 |
C1—N1—Cu1 | 120.0 (1) | C3—C4—H4 | 120.5 |
N1—C1—C2 | 123.7 (2) | N1—C5—H5 | 118.3 |
C1—C2—C3 | 118.8 (2) | C4—C5—H5 | 118.3 |
C4—C3—C2 | 118.0 (2) | C7—C6—H6a | 109.8 |
C4—C3—S1 | 126.2 (2) | S1—C6—H6a | 109.8 |
C2—C3—S1 | 115.9 (2) | C7—C6—H6b | 109.8 |
C5—C4—C3 | 119.1 (2) | S1—C6—H6b | 109.8 |
N1—C5—C4 | 123.4 (2) | H6a—C6—H6b | 108.2 |
| | | |
N2i—Cu1—N1—C5 | −133.8 (2) | C1—C2—C3—S1 | −179.3 (1) |
N2—Cu1—N1—C5 | 46.2 (2) | C6—S1—C3—C4 | −2.0 (2) |
O1wi—Cu1—N1—C5 | −50.2 (1) | C6—S1—C3—C2 | 178.5 (1) |
O1w—Cu1—N1—C5 | 129.8 (1) | C2—C3—C4—C5 | −0.7 (3) |
N2i—Cu1—N1—C1 | 49.5 (1) | S1—C3—C4—C5 | 179.8 (2) |
N2—Cu1—N1—C1 | −130.5 (1) | C1—N1—C5—C4 | 1.4 (3) |
O1wi—Cu1—N1—C1 | 133.1 (1) | Cu1—N1—C5—C4 | −175.4 (1) |
O1w—Cu1—N1—C1 | −46.9 (1) | C3—C4—C5—N1 | −0.6 (3) |
C5—N1—C1—C2 | −0.9 (3) | C3—S1—C6—C7 | −179.9 (1) |
Cu1—N1—C1—C2 | 176.0 (1) | S1—C6—C7—O1 | 179.0 (1) |
N1—C1—C2—C3 | −0.4 (3) | S1—C6—C7—O2 | −1.6 (2) |
C1—C2—C3—C4 | 1.2 (3) | | |
Symmetry code: (i) −x+1/2, −y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2n2···O1ii | 0.88 (1) | 2.40 (1) | 3.267 (2) | 167 (2) |
N2—H2n1···O2iii | 0.89 (1) | 2.20 (1) | 3.092 (2) | 178 (2) |
N2—H2n3···O1iv | 0.89 (1) | 2.16 (1) | 3.045 (2) | 177 (2) |
O1w—H1w1···O1iii | 0.83 (1) | 1.98 (1) | 2.790 (2) | 164 (2) |
O1w—H1w2···O2ii | 0.82 (1) | 2.01 (1) | 2.828 (2) | 176 (2) |
Symmetry codes: (ii) x+1/2, y+1/2, z; (iii) −x, −y+1, −z; (iv) −x, y, −z−1/2. |