Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100012488/qa0355sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100012488/qa0355Isup2.hkl |
CCDC reference: 152659
Equimolar (dmpda)Pt(isonic)2 (1.0 g, 1.85 mmol) and Cu(NO3)2·3H2O (0.45 g, 1.85 mmol) were dissolved in water (10 ml) and acetone (5 ml) was added to the solution. After two weeks at room temperature, blue block-shaped crystals had formed and were filtered off and washed with cold water and acetone.
Water atoms were not located; others were included in the structure-factor calculations using a riding model. The largest difference map features lie close to the Pt atom.
Data collection: CAD-4-VAX (Enraf-Nonius, 1981); cell refinement: CAD-4-VAX; data reduction: SDP (Frenz, 1985); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.
[CuPt(C6H4NO2)2(C5H14N2)(H2O)3](NO3)2 | F(000) = 1612 |
Mr = 819.12 | Dx = 1.957 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 10.105 (3) Å | Cell parameters from 25 reflections |
b = 18.133 (3) Å | θ = 9.4–14.2° |
c = 15.590 (5) Å | µ = 5.87 mm−1 |
β = 103.29 (2)° | T = 293 K |
V = 2780.1 (12) Å3 | Block, blue |
Z = 4 | 0.55 × 0.40 × 0.35 mm |
Enraf-Nonius CAD-4 diffractometer | 4175 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.035 |
Graphite monochromator | θmax = 25.0°, θmin = 1.8° |
ω/2θ scans | h = 0→11 |
Absorption correction: ψ scan (North et al., 1968) | k = −21→21 |
Tmin = 0.058, Tmax = 0.128 | l = −18→18 |
6863 measured reflections | 3 standard reflections every 120 min |
4819 independent reflections | intensity decay: 9.6% |
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) = 0.091 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0497P)2 + 7.8145P] where P = (Fo2 + 2Fc2)/3 |
4819 reflections | (Δ/σ)max = 0.011 |
361 parameters | Δρmax = 2.34 e Å−3 |
0 restraints | Δρmin = −1.29 e Å−3 |
[CuPt(C6H4NO2)2(C5H14N2)(H2O)3](NO3)2 | V = 2780.1 (12) Å3 |
Mr = 819.12 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.105 (3) Å | µ = 5.87 mm−1 |
b = 18.133 (3) Å | T = 293 K |
c = 15.590 (5) Å | 0.55 × 0.40 × 0.35 mm |
β = 103.29 (2)° |
Enraf-Nonius CAD-4 diffractometer | 4175 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.035 |
Tmin = 0.058, Tmax = 0.128 | 3 standard reflections every 120 min |
6863 measured reflections | intensity decay: 9.6% |
4819 independent reflections |
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.07 | Δρmax = 2.34 e Å−3 |
4819 reflections | Δρmin = −1.29 e Å−3 |
361 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Pt | 0.72126 (2) | 0.788103 (11) | 0.956049 (13) | 0.02456 (9) | |
Cu | 0.28860 (7) | 0.98180 (4) | 1.33338 (5) | 0.02985 (17) | |
O1 | 0.3289 (4) | 0.5315 (2) | 1.1042 (3) | 0.0383 (10) | |
O2 | 0.2006 (5) | 0.5370 (3) | 0.9669 (3) | 0.0484 (13) | |
O3 | 0.3959 (5) | 0.9309 (2) | 1.2660 (3) | 0.0361 (10) | |
O4 | 0.2976 (6) | 1.0010 (3) | 1.1531 (4) | 0.0647 (16) | |
O5 | 0.1403 (5) | 0.9089 (2) | 1.2935 (3) | 0.0394 (10) | |
O6 | 0.4161 (5) | 1.0662 (3) | 1.3502 (4) | 0.0511 (13) | |
O7 | 0.4099 (5) | 0.9195 (2) | 1.4553 (3) | 0.0393 (10) | |
N1 | 0.5977 (5) | 0.7007 (3) | 0.9657 (3) | 0.0291 (11) | |
H1A | 0.6057 | 0.7476 | 0.9852 | 0.035* | |
H1B | 0.6610 | 0.6940 | 0.9342 | 0.035* | |
N2 | 0.6148 (5) | 0.8446 (3) | 1.0310 (3) | 0.0290 (11) | |
H2A | 0.6910 | 0.8627 | 1.0183 | 0.035* | |
H2B | 0.5995 | 0.8002 | 1.0048 | 0.035* | |
N3 | 0.8181 (5) | 0.7281 (3) | 0.8790 (3) | 0.0310 (11) | |
N4 | 0.8378 (5) | 0.8797 (3) | 0.9522 (3) | 0.0307 (11) | |
C1 | 0.4761 (7) | 0.6939 (4) | 0.9107 (4) | 0.0355 (14) | |
H1 | 0.4556 | 0.7228 | 0.8602 | 0.043* | |
C2 | 0.3799 (6) | 0.6452 (4) | 0.9266 (4) | 0.0366 (14) | |
H2 | 0.2956 | 0.6414 | 0.8873 | 0.044* | |
C3 | 0.4100 (6) | 0.6019 (3) | 1.0016 (4) | 0.0288 (12) | |
C4 | 0.5374 (6) | 0.6075 (3) | 1.0563 (4) | 0.0358 (14) | |
H4 | 0.5611 | 0.5783 | 1.1066 | 0.043* | |
C5 | 0.6292 (6) | 0.6565 (3) | 1.0361 (4) | 0.0359 (14) | |
H5 | 0.7160 | 0.6590 | 1.0726 | 0.043* | |
C6 | 0.3026 (6) | 0.5525 (3) | 1.0250 (4) | 0.0318 (13) | |
C7 | 0.6409 (6) | 0.8334 (3) | 1.1190 (4) | 0.0337 (13) | |
H7 | 0.7112 | 0.8019 | 1.1452 | 0.040* | |
C8 | 0.5659 (7) | 0.8674 (3) | 1.1703 (4) | 0.0362 (14) | |
H8 | 0.5865 | 0.8600 | 1.2309 | 0.043* | |
C9 | 0.4592 (6) | 0.9128 (3) | 1.1310 (4) | 0.0286 (12) | |
C10 | 0.4323 (7) | 0.9234 (3) | 1.0416 (4) | 0.0352 (14) | |
H10 | 0.3609 | 0.9536 | 1.0139 | 0.042* | |
C11 | 0.5125 (6) | 0.8887 (3) | 0.9934 (4) | 0.0336 (13) | |
H11 | 0.4946 | 0.8963 | 0.9328 | 0.040* | |
C12 | 0.3754 (6) | 0.9522 (3) | 1.1861 (4) | 0.0331 (13) | |
C13 | 0.9640 (6) | 0.7410 (3) | 0.8849 (4) | 0.0347 (14) | |
H13A | 0.9922 | 0.7106 | 0.8412 | 0.042* | |
H13B | 1.0146 | 0.7249 | 0.9424 | 0.042* | |
C14 | 1.0031 (6) | 0.8211 (3) | 0.8714 (4) | 0.0355 (14) | |
C15 | 0.9831 (6) | 0.8697 (3) | 0.9473 (4) | 0.0368 (14) | |
H15A | 1.0331 | 0.8483 | 1.0022 | 0.044* | |
H15B | 1.0221 | 0.9178 | 0.9415 | 0.044* | |
C16 | 1.1574 (8) | 0.8195 (5) | 0.8754 (7) | 0.064 (2) | |
H16A | 1.1883 | 0.8685 | 0.8672 | 0.097* | |
H16B | 1.1745 | 0.7880 | 0.8297 | 0.097* | |
H16C | 1.2051 | 0.8011 | 0.9317 | 0.097* | |
C17 | 0.9257 (9) | 0.8513 (4) | 0.7833 (5) | 0.054 (2) | |
H17A | 0.9526 | 0.9014 | 0.7772 | 0.081* | |
H17B | 0.8299 | 0.8495 | 0.7805 | 0.081* | |
H17C | 0.9457 | 0.8220 | 0.7365 | 0.081* | |
N5 | 0.1528 (7) | 0.0299 (4) | 0.8240 (4) | 0.0517 (16) | |
N6 | 0.8329 (11) | 0.2478 (4) | 0.8557 (7) | 0.094 (3) | |
O8 | 0.1134 (6) | 0.0335 (4) | 0.7424 (3) | 0.0653 (16) | |
O9 | 0.2581 (7) | −0.0041 (4) | 0.8548 (5) | 0.081 (2) | |
O10 | 0.0857 (8) | 0.0594 (5) | 0.8702 (4) | 0.098 (3) | |
O11 | 0.8497 (13) | 0.2960 (4) | 0.9061 (6) | 0.139 (5) | |
O12 | 0.7950 (12) | 0.1886 (5) | 0.8507 (8) | 0.158 (5) | |
O13 | 0.8774 (12) | 0.2605 (9) | 0.7898 (8) | 0.155 (5) | |
OW1 | 0.6567 (6) | 0.0487 (3) | 0.3034 (4) | 0.0654 (15) | |
OW2 | 0.6303 (9) | 0.2089 (4) | 0.2788 (6) | 0.097 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt | 0.02856 (14) | 0.02250 (13) | 0.02683 (14) | −0.00271 (8) | 0.01506 (10) | −0.00061 (8) |
Cu | 0.0335 (4) | 0.0284 (4) | 0.0316 (4) | 0.0068 (3) | 0.0156 (3) | −0.0029 (3) |
O1 | 0.035 (2) | 0.047 (3) | 0.034 (2) | −0.013 (2) | 0.013 (2) | 0.0088 (19) |
O2 | 0.037 (3) | 0.066 (3) | 0.041 (3) | −0.023 (2) | 0.007 (2) | 0.009 (2) |
O3 | 0.044 (3) | 0.035 (2) | 0.034 (2) | 0.0094 (19) | 0.018 (2) | −0.0025 (18) |
O4 | 0.080 (4) | 0.066 (3) | 0.056 (3) | 0.042 (3) | 0.030 (3) | 0.014 (3) |
O5 | 0.041 (3) | 0.040 (2) | 0.039 (2) | −0.001 (2) | 0.012 (2) | −0.0031 (19) |
O6 | 0.053 (3) | 0.037 (3) | 0.069 (3) | −0.006 (2) | 0.027 (3) | −0.011 (2) |
O7 | 0.045 (3) | 0.034 (2) | 0.036 (2) | 0.007 (2) | 0.004 (2) | −0.0033 (18) |
N1 | 0.035 (3) | 0.028 (2) | 0.031 (3) | −0.005 (2) | 0.021 (2) | −0.002 (2) |
N2 | 0.030 (3) | 0.026 (2) | 0.036 (3) | −0.002 (2) | 0.017 (2) | 0.001 (2) |
N3 | 0.034 (3) | 0.027 (2) | 0.039 (3) | −0.008 (2) | 0.023 (2) | −0.007 (2) |
N4 | 0.033 (3) | 0.025 (2) | 0.038 (3) | −0.003 (2) | 0.017 (2) | −0.001 (2) |
C1 | 0.037 (4) | 0.041 (3) | 0.029 (3) | −0.007 (3) | 0.009 (3) | 0.007 (3) |
C2 | 0.029 (3) | 0.046 (4) | 0.033 (3) | −0.008 (3) | 0.003 (3) | 0.008 (3) |
C3 | 0.028 (3) | 0.029 (3) | 0.034 (3) | −0.002 (2) | 0.016 (3) | 0.001 (2) |
C4 | 0.034 (3) | 0.037 (3) | 0.036 (3) | −0.005 (3) | 0.007 (3) | 0.010 (3) |
C5 | 0.026 (3) | 0.036 (3) | 0.045 (4) | −0.006 (2) | 0.006 (3) | 0.011 (3) |
C6 | 0.032 (3) | 0.034 (3) | 0.033 (3) | −0.007 (3) | 0.014 (3) | 0.001 (3) |
C7 | 0.036 (3) | 0.037 (3) | 0.031 (3) | 0.011 (3) | 0.014 (3) | 0.006 (3) |
C8 | 0.045 (4) | 0.038 (3) | 0.030 (3) | 0.010 (3) | 0.017 (3) | 0.003 (3) |
C9 | 0.034 (3) | 0.029 (3) | 0.027 (3) | 0.000 (2) | 0.015 (2) | −0.002 (2) |
C10 | 0.033 (3) | 0.039 (3) | 0.035 (3) | 0.004 (3) | 0.013 (3) | 0.003 (3) |
C11 | 0.039 (3) | 0.038 (3) | 0.027 (3) | 0.001 (3) | 0.012 (3) | −0.002 (2) |
C12 | 0.032 (3) | 0.030 (3) | 0.041 (4) | 0.008 (3) | 0.016 (3) | 0.000 (3) |
C13 | 0.033 (3) | 0.031 (3) | 0.044 (4) | 0.002 (3) | 0.017 (3) | −0.004 (3) |
C14 | 0.032 (3) | 0.033 (3) | 0.047 (4) | −0.006 (3) | 0.021 (3) | −0.001 (3) |
C15 | 0.036 (3) | 0.032 (3) | 0.044 (4) | −0.005 (3) | 0.011 (3) | −0.003 (3) |
C16 | 0.042 (4) | 0.049 (4) | 0.113 (7) | −0.011 (4) | 0.042 (5) | −0.008 (5) |
C17 | 0.079 (6) | 0.050 (4) | 0.039 (4) | −0.003 (4) | 0.025 (4) | 0.007 (3) |
N5 | 0.048 (4) | 0.060 (4) | 0.044 (4) | −0.022 (3) | 0.003 (3) | 0.001 (3) |
N6 | 0.118 (8) | 0.045 (4) | 0.085 (6) | −0.014 (5) | −0.044 (6) | 0.015 (4) |
O8 | 0.052 (3) | 0.100 (5) | 0.041 (3) | 0.019 (3) | 0.006 (3) | −0.002 (3) |
O9 | 0.065 (4) | 0.072 (4) | 0.090 (5) | −0.013 (3) | −0.018 (4) | 0.029 (4) |
O10 | 0.085 (5) | 0.159 (7) | 0.053 (4) | −0.026 (5) | 0.022 (4) | −0.040 (4) |
O11 | 0.243 (13) | 0.067 (5) | 0.073 (5) | 0.011 (6) | −0.032 (7) | −0.015 (4) |
O12 | 0.172 (11) | 0.077 (6) | 0.190 (11) | −0.034 (7) | −0.030 (9) | −0.004 (7) |
O13 | 0.113 (8) | 0.238 (14) | 0.101 (8) | −0.005 (9) | −0.002 (7) | 0.023 (9) |
OW1 | 0.050 (3) | 0.068 (4) | 0.081 (4) | 0.001 (3) | 0.022 (3) | −0.004 (3) |
OW2 | 0.091 (6) | 0.100 (6) | 0.099 (6) | −0.014 (4) | 0.019 (5) | 0.020 (4) |
Pt—N3 | 2.031 (5) | C1—C2 | 1.377 (8) |
Pt—N2 | 2.037 (5) | C2—C3 | 1.382 (8) |
Pt—N4 | 2.044 (5) | C3—C4 | 1.375 (9) |
Pt—N1 | 2.044 (5) | C3—C6 | 1.516 (8) |
Cu—O3 | 1.912 (4) | C4—C5 | 1.372 (8) |
Cu—O1i | 1.924 (4) | C7—C8 | 1.368 (8) |
Cu—O6 | 1.978 (5) | C8—C9 | 1.383 (9) |
Cu—O5 | 1.988 (5) | C9—C10 | 1.371 (8) |
Cu—O7 | 2.306 (4) | C9—C12 | 1.516 (8) |
O1—C6 | 1.260 (7) | C10—C11 | 1.377 (8) |
O1—Cuii | 1.924 (4) | C13—C14 | 1.531 (9) |
O2—C6 | 1.239 (7) | C14—C17 | 1.518 (10) |
O3—C12 | 1.275 (7) | C14—C15 | 1.525 (9) |
O4—C12 | 1.218 (8) | C14—C16 | 1.546 (9) |
N1—C1 | 1.333 (8) | N5—O10 | 1.220 (9) |
N1—C5 | 1.338 (8) | N5—O9 | 1.228 (9) |
N2—C11 | 1.332 (8) | N5—O8 | 1.244 (8) |
N2—C7 | 1.351 (7) | N6—O12 | 1.136 (12) |
N3—C13 | 1.476 (8) | N6—O11 | 1.161 (11) |
N4—C15 | 1.500 (8) | N6—O13 | 1.235 (15) |
N3—Pt—N2 | 176.76 (19) | C2—C3—C6 | 120.6 (5) |
N3—Pt—N4 | 93.41 (19) | C5—C4—C3 | 119.4 (6) |
N2—Pt—N4 | 89.53 (19) | N1—C5—C4 | 122.1 (6) |
N3—Pt—N1 | 90.74 (19) | O2—C6—O1 | 126.9 (5) |
N2—Pt—N1 | 86.32 (19) | O2—C6—C3 | 118.6 (5) |
N4—Pt—N1 | 175.84 (18) | O1—C6—C3 | 114.5 (5) |
O3—Cu—O1i | 176.6 (2) | N2—C7—C8 | 121.4 (6) |
O3—Cu—O6 | 90.7 (2) | C7—C8—C9 | 119.4 (6) |
O1i—Cu—O6 | 91.7 (2) | C10—C9—C8 | 119.0 (5) |
O3—Cu—O5 | 89.37 (19) | C10—C9—C12 | 120.3 (5) |
O1i—Cu—O5 | 87.78 (19) | C8—C9—C12 | 120.7 (5) |
O6—Cu—O5 | 167.6 (2) | C9—C10—C11 | 119.2 (6) |
O3—Cu—O7 | 87.42 (17) | N2—C11—C10 | 121.9 (6) |
O1i—Cu—O7 | 94.88 (17) | O4—C12—O3 | 125.3 (6) |
O6—Cu—O7 | 93.6 (2) | O4—C12—C9 | 119.5 (6) |
O5—Cu—O7 | 98.75 (18) | O3—C12—C9 | 115.1 (5) |
C6—O1—Cuii | 128.4 (4) | N3—C13—C14 | 115.4 (5) |
C12—O3—Cu | 113.9 (4) | C17—C14—C15 | 111.1 (6) |
C1—N1—C5 | 118.8 (5) | C17—C14—C13 | 111.8 (6) |
C1—N1—Pt | 120.9 (4) | C15—C14—C13 | 110.9 (5) |
C5—N1—Pt | 119.4 (4) | C17—C14—C16 | 110.4 (6) |
C11—N2—C7 | 119.2 (5) | C15—C14—C16 | 106.9 (6) |
C11—N2—Pt | 120.5 (4) | C13—C14—C16 | 105.5 (5) |
C7—N2—Pt | 120.1 (4) | N4—C15—C14 | 114.6 (5) |
C13—N3—Pt | 119.2 (4) | O10—N5—O9 | 122.6 (8) |
C15—N4—Pt | 118.7 (4) | O10—N5—O8 | 119.3 (7) |
N1—C1—C2 | 121.9 (6) | O9—N5—O8 | 118.1 (7) |
C1—C2—C3 | 119.2 (6) | O12—N6—O11 | 138.8 (15) |
C4—C3—C2 | 118.5 (5) | O12—N6—O13 | 107.4 (13) |
C4—C3—C6 | 120.9 (5) | O11—N6—O13 | 113.5 (12) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+5/2; (ii) −x+1/2, y−1/2, −z+5/2. |
Experimental details
Crystal data | |
Chemical formula | [CuPt(C6H4NO2)2(C5H14N2)(H2O)3](NO3)2 |
Mr | 819.12 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 10.105 (3), 18.133 (3), 15.590 (5) |
β (°) | 103.29 (2) |
V (Å3) | 2780.1 (12) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.87 |
Crystal size (mm) | 0.55 × 0.40 × 0.35 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.058, 0.128 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6863, 4819, 4175 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.091, 1.07 |
No. of reflections | 4819 |
No. of parameters | 361 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.34, −1.29 |
Computer programs: CAD-4-VAX (Enraf-Nonius, 1981), CAD-4-VAX, SDP (Frenz, 1985), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97.
The title compound, (I), has been found to be a one-dimensional coordination polymer of the zigzag-type. The polymer has repeat units in which the Cu—Pt—Cu' angle is 64.9°. One Cu atom links two platinum complex molecules through coordination to two carboxylate groups from the two platinum complex units. Three water molecules are also bound to the Cu atom forming a square-pyramidal geometry. The axial water molecule has a bond to the Cu atom of 2.306 (4) Å, whereas carboxylate O atoms and two equatorial water molecules have distances from copper in the range 1.912 (4)–1.988 (5) Å, which is similar to the pattern in other copper compounds (Shields et al., 1972). The structural properties of the platinum complex moiety, (dmpda)Pt(isonic)2, are similar to those of the starting platinum complex, whose structure was previously reported (Song et al., 1999).