Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106047306/bk5045sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106047306/bk5045NiL20sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106047306/bk5045CuL20sup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106047306/bk5045PdL20sup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106047306/bk5045PtL20sup5.hkl |
CCDC references: 637760; 637761; 637762; 637763
Data collection: Bruker SMART (Bruker AXS,1998) for NiL20; Bruker SMART for CuL20, PdL20, PtL20. Cell refinement: Bruker SMART (Bruker AXS,1998) for NiL20; Bruker SMART for CuL20, PdL20, PtL20. Data reduction: Bruker SHELXTL (Sheldrick,2001) for NiL20; Bruker SHELXTL for CuL20, PdL20, PtL20. Program(s) used to solve structure: Bruker SHELXTL (Sheldrick,2001) for NiL20; Bruker SHELXTL for CuL20, PdL20, PtL20. Program(s) used to refine structure: Bruker SHELXTL (Sheldrick,2001) for NiL20; Bruker SHELXTL for CuL20, PdL20, PtL20. Molecular graphics: Bruker SHELXTL (Sheldrick,2001) for NiL20; Bruker SHELXTL for CuL20, PdL20, PtL20. For all compounds, software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).
C22H30N6NiS2 | Dx = 1.413 Mg m−3 |
Mr = 501.35 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P41212 | Cell parameters from 12044 reflections |
a = 10.2852 (3) Å | θ = 2.7–31.0° |
c = 22.2862 (13) Å | µ = 1.02 mm−1 |
V = 2357.55 (17) Å3 | T = 118 K |
Z = 4 | Quadratic bi-pyramidal shaped, brown |
F(000) = 1056 | 0.50 × 0.30 × 0.05 mm |
CCD area detector diffractometer | 3630 independent reflections |
Radiation source: fine-focus sealed tube | 3436 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
Detector resolution: 8.192 pixels mm-1 | θmax = 31.0°, θmin = 2.2° |
ω scans | h = −13→14 |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | k = −14→14 |
Tmin = 0.74, Tmax = 0.96 | l = −31→30 |
31608 measured reflections |
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)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.078 | w = 1/[σ2(Fo2) + (0.0407P)2 + 0.3442P] where P = (Fo2 + 2Fc2)/3 |
S = 1.16 | (Δ/σ)max = 0.001 |
3630 reflections | Δρmax = 0.61 e Å−3 |
201 parameters | Δρmin = −0.26 e Å−3 |
0 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.021 (12) |
C22H30N6NiS2 | Z = 4 |
Mr = 501.35 | Mo Kα radiation |
Tetragonal, P41212 | µ = 1.02 mm−1 |
a = 10.2852 (3) Å | T = 118 K |
c = 22.2862 (13) Å | 0.50 × 0.30 × 0.05 mm |
V = 2357.55 (17) Å3 |
CCD area detector diffractometer | 3630 independent reflections |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | 3436 reflections with I > 2σ(I) |
Tmin = 0.74, Tmax = 0.96 | Rint = 0.043 |
31608 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.078 | Δρmax = 0.61 e Å−3 |
S = 1.16 | Δρmin = −0.26 e Å−3 |
3630 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
201 parameters | Absolute structure parameter: 0.021 (12) |
0 restraints |
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 | ||
Ni | 0.14902 (2) | 0.14902 (2) | 0.0000 | 0.01454 (8) | |
S | −0.01504 (4) | 0.16012 (4) | 0.06373 (2) | 0.01851 (10) | |
N1 | 0.07768 (13) | 0.29876 (13) | −0.03467 (6) | 0.0129 (3) | |
N2 | −0.03902 (13) | 0.34689 (14) | −0.02047 (6) | 0.0142 (3) | |
N3 | −0.20611 (14) | 0.33344 (15) | 0.04815 (6) | 0.0169 (3) | |
C1 | −0.09112 (16) | 0.28819 (16) | 0.02852 (7) | 0.0138 (3) | |
C2 | −0.27465 (17) | 0.44026 (18) | 0.01804 (8) | 0.0191 (4) | |
H2A | −0.2119 | 0.4955 | −0.0021 | 0.023* | |
H2B | −0.3196 | 0.4925 | 0.0478 | 0.023* | |
C3 | −0.3721 (2) | 0.3900 (2) | −0.02740 (9) | 0.0263 (4) | |
H3A | −0.4151 | 0.4621 | −0.0462 | 0.039* | |
H3B | −0.4352 | 0.3365 | −0.0075 | 0.039* | |
H3C | −0.3277 | 0.3395 | −0.0573 | 0.039* | |
C4 | −0.27118 (18) | 0.2763 (2) | 0.10021 (8) | 0.0210 (4) | |
H4A | −0.2535 | 0.1837 | 0.1013 | 0.025* | |
H4B | −0.3644 | 0.2879 | 0.0961 | 0.025* | |
C5 | −0.2266 (2) | 0.3375 (3) | 0.15886 (9) | 0.0325 (5) | |
H5A | −0.2714 | 0.2973 | 0.1918 | 0.049* | |
H5B | −0.2456 | 0.4289 | 0.1583 | 0.049* | |
H5C | −0.1347 | 0.3249 | 0.1635 | 0.049* | |
C6 | 0.13032 (15) | 0.35289 (16) | −0.08777 (7) | 0.0136 (3) | |
C7 | 0.05541 (18) | 0.41279 (17) | −0.13203 (8) | 0.0180 (3) | |
H7 | −0.0337 | 0.4227 | −0.1267 | 0.022* | |
C8 | 0.11433 (19) | 0.45755 (18) | −0.18413 (9) | 0.0219 (4) | |
H8 | 0.0641 | 0.4958 | −0.2140 | 0.026* | |
C9 | 0.24787 (19) | 0.44559 (18) | −0.19198 (9) | 0.0219 (4) | |
H9 | 0.2868 | 0.4761 | −0.2269 | 0.026* | |
C10 | 0.32319 (17) | 0.38794 (17) | −0.14757 (8) | 0.0193 (4) | |
H10 | 0.4127 | 0.3810 | −0.1526 | 0.023* | |
C11 | 0.26524 (16) | 0.34072 (17) | −0.09572 (8) | 0.0161 (3) | |
H11 | 0.3157 | 0.3011 | −0.0663 | 0.019* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni | 0.01353 (10) | 0.01353 (10) | 0.01657 (15) | 0.00528 (11) | −0.00051 (8) | 0.00051 (8) |
S | 0.01692 (19) | 0.0200 (2) | 0.0186 (2) | 0.00595 (16) | 0.00190 (15) | 0.00582 (17) |
N1 | 0.0119 (6) | 0.0121 (6) | 0.0146 (7) | 0.0022 (5) | −0.0013 (5) | −0.0006 (5) |
N2 | 0.0108 (6) | 0.0150 (6) | 0.0169 (6) | 0.0035 (5) | 0.0008 (5) | 0.0000 (6) |
N3 | 0.0133 (6) | 0.0196 (7) | 0.0177 (7) | 0.0042 (5) | 0.0025 (5) | 0.0028 (6) |
C1 | 0.0126 (7) | 0.0148 (7) | 0.0142 (8) | 0.0018 (6) | −0.0016 (6) | −0.0007 (6) |
C2 | 0.0150 (8) | 0.0188 (8) | 0.0235 (9) | 0.0067 (6) | 0.0032 (7) | 0.0015 (7) |
C3 | 0.0301 (11) | 0.0274 (9) | 0.0214 (9) | 0.0130 (8) | −0.0049 (8) | −0.0004 (8) |
C4 | 0.0147 (9) | 0.0277 (10) | 0.0206 (8) | 0.0023 (6) | 0.0049 (7) | 0.0038 (8) |
C5 | 0.0294 (10) | 0.0487 (14) | 0.0194 (9) | 0.0000 (10) | 0.0022 (8) | 0.0008 (10) |
C6 | 0.0146 (7) | 0.0113 (6) | 0.0151 (7) | 0.0004 (6) | 0.0003 (6) | −0.0016 (6) |
C7 | 0.0161 (8) | 0.0172 (8) | 0.0208 (9) | 0.0030 (6) | 0.0000 (7) | −0.0002 (7) |
C8 | 0.0275 (9) | 0.0197 (8) | 0.0184 (8) | 0.0030 (7) | −0.0005 (7) | 0.0034 (7) |
C9 | 0.0295 (10) | 0.0158 (9) | 0.0205 (9) | −0.0016 (7) | 0.0079 (8) | −0.0008 (7) |
C10 | 0.0162 (8) | 0.0154 (8) | 0.0262 (9) | −0.0016 (6) | 0.0054 (7) | −0.0048 (7) |
C11 | 0.0153 (7) | 0.0144 (8) | 0.0187 (8) | 0.0011 (6) | 0.0003 (6) | −0.0018 (7) |
Ni—N1i | 1.8728 (14) | C4—C5 | 1.521 (3) |
Ni—N1 | 1.8728 (14) | C4—H4A | 0.9700 |
Ni—Si | 2.2085 (4) | C4—H4B | 0.9700 |
Ni—S | 2.2085 (4) | C5—H5A | 0.9600 |
S—C1 | 1.7213 (17) | C5—H5B | 0.9600 |
N1—N2 | 1.3363 (19) | C5—H5C | 0.9600 |
N1—C6 | 1.415 (2) | C6—C7 | 1.395 (2) |
N2—C1 | 1.358 (2) | C6—C11 | 1.405 (2) |
N3—C1 | 1.344 (2) | C7—C8 | 1.388 (2) |
N3—C4 | 1.463 (2) | C7—H7 | 0.9300 |
N3—C2 | 1.468 (2) | C8—C9 | 1.390 (3) |
C2—C3 | 1.515 (3) | C8—H8 | 0.9300 |
C2—H2A | 0.9700 | C9—C10 | 1.390 (3) |
C2—H2B | 0.9700 | C9—H9 | 0.9300 |
C3—H3A | 0.9600 | C10—C11 | 1.388 (2) |
C3—H3B | 0.9600 | C10—H10 | 0.9300 |
C3—H3C | 0.9600 | C11—H11 | 0.9300 |
N1i—Ni—N1 | 144.55 (9) | N3—C4—H4A | 109.2 |
N1i—Ni—Si | 85.61 (4) | C5—C4—H4A | 109.2 |
N1—Ni—Si | 112.53 (4) | N3—C4—H4B | 109.2 |
N1i—Ni—S | 112.53 (4) | C5—C4—H4B | 109.2 |
N1—Ni—S | 85.61 (4) | H4A—C4—H4B | 107.9 |
Si—Ni—S | 119.50 (3) | C4—C5—H5A | 109.5 |
C1—S—Ni | 95.38 (6) | C4—C5—H5B | 109.5 |
N2—N1—C6 | 113.32 (13) | H5A—C5—H5B | 109.5 |
N2—N1—Ni | 123.97 (11) | C4—C5—H5C | 109.5 |
C6—N1—Ni | 121.23 (11) | H5A—C5—H5C | 109.5 |
N1—N2—C1 | 112.35 (13) | H5B—C5—H5C | 109.5 |
C1—N3—C4 | 121.45 (15) | C7—C6—C11 | 119.72 (16) |
C1—N3—C2 | 122.21 (14) | C7—C6—N1 | 123.62 (15) |
C4—N3—C2 | 116.32 (14) | C11—C6—N1 | 116.64 (15) |
N3—C1—N2 | 117.06 (14) | C8—C7—C6 | 119.79 (17) |
N3—C1—S | 121.11 (13) | C8—C7—H7 | 120.1 |
N2—C1—S | 121.83 (12) | C6—C7—H7 | 120.1 |
N3—C2—C3 | 111.58 (16) | C9—C8—C7 | 120.49 (18) |
N3—C2—H2A | 109.3 | C9—C8—H8 | 119.8 |
C3—C2—H2A | 109.3 | C7—C8—H8 | 119.8 |
N3—C2—H2B | 109.3 | C8—C9—C10 | 119.92 (17) |
C3—C2—H2B | 109.3 | C8—C9—H9 | 120.0 |
H2A—C2—H2B | 108.0 | C10—C9—H9 | 120.0 |
C2—C3—H3A | 109.5 | C11—C10—C9 | 120.19 (17) |
C2—C3—H3B | 109.5 | C11—C10—H10 | 119.9 |
H3A—C3—H3B | 109.5 | C9—C10—H10 | 119.9 |
C2—C3—H3C | 109.5 | C10—C11—C6 | 119.88 (16) |
H3A—C3—H3C | 109.5 | C10—C11—H11 | 120.1 |
H3B—C3—H3C | 109.5 | C6—C11—H11 | 120.1 |
N3—C4—C5 | 112.19 (17) | ||
N1i—Ni—S—C1 | 153.90 (8) | Ni—S—C1—N2 | −2.51 (14) |
N1—Ni—S—C1 | 5.38 (7) | C1—N3—C2—C3 | 93.7 (2) |
Si—Ni—S—C1 | −108.08 (6) | C4—N3—C2—C3 | −85.0 (2) |
N1i—Ni—N1—N2 | −133.45 (13) | C1—N3—C4—C5 | 87.1 (2) |
Si—Ni—N1—N2 | 110.45 (12) | C2—N3—C4—C5 | −94.2 (2) |
S—Ni—N1—N2 | −9.75 (12) | N2—N1—C6—C7 | −21.5 (2) |
N1i—Ni—N1—C6 | 61.33 (12) | Ni—N1—C6—C7 | 145.13 (14) |
Si—Ni—N1—C6 | −54.77 (13) | N2—N1—C6—C11 | 160.30 (15) |
S—Ni—N1—C6 | −174.97 (12) | Ni—N1—C6—C11 | −33.0 (2) |
C6—N1—N2—C1 | 176.32 (13) | C11—C6—C7—C8 | 1.3 (3) |
Ni—N1—N2—C1 | 10.06 (19) | N1—C6—C7—C8 | −176.80 (16) |
C4—N3—C1—N2 | 179.44 (16) | C6—C7—C8—C9 | −1.4 (3) |
C2—N3—C1—N2 | 0.8 (2) | C7—C8—C9—C10 | 0.3 (3) |
C4—N3—C1—S | 0.2 (2) | C8—C9—C10—C11 | 0.8 (3) |
C2—N3—C1—S | −178.39 (14) | C9—C10—C11—C6 | −0.9 (3) |
N1—N2—C1—N3 | 177.19 (14) | C7—C6—C11—C10 | −0.2 (3) |
N1—N2—C1—S | −3.6 (2) | N1—C6—C11—C10 | 178.04 (15) |
Ni—S—C1—N3 | 176.68 (13) |
Symmetry code: (i) y, x, −z. |
C22H30CuN6S2 | Dx = 1.428 Mg m−3 |
Mr = 506.18 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P41212 | Cell parameters from 10241 reflections |
a = 10.2643 (4) Å | θ = 2.7–28.0° |
c = 22.3519 (13) Å | µ = 1.13 mm−1 |
V = 2354.90 (19) Å3 | T = 118 K |
Z = 4 | Quadratic bi-pyramidal shaped, black |
F(000) = 1060 | 0.40 × 0.35 × 0.15 mm |
CCD area detector diffractometer | 2832 independent reflections |
Radiation source: fine-focus sealed tube | 2788 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 8.192 pixels mm-1 | θmax = 28.0°, θmin = 2.2° |
ω scans | h = −13→12 |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | k = −13→13 |
Tmin = 0.661, Tmax = 0.849 | l = −28→28 |
16807 measured reflections |
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-atom parameters constrained |
wR(F2) = 0.070 | w = 1/[σ2(Fo2) + (0.P)2 + 0.1079P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max < 0.001 |
2832 reflections | Δρmax = 0.36 e Å−3 |
141 parameters | Δρmin = −0.18 e Å−3 |
0 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 1132 Fridel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.012 (9) |
C22H30CuN6S2 | Z = 4 |
Mr = 506.18 | Mo Kα radiation |
Tetragonal, P41212 | µ = 1.13 mm−1 |
a = 10.2643 (4) Å | T = 118 K |
c = 22.3519 (13) Å | 0.40 × 0.35 × 0.15 mm |
V = 2354.90 (19) Å3 |
CCD area detector diffractometer | 2832 independent reflections |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | 2788 reflections with I > 2σ(I) |
Tmin = 0.661, Tmax = 0.849 | Rint = 0.027 |
16807 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
wR(F2) = 0.070 | Δρmax = 0.36 e Å−3 |
S = 1.10 | Δρmin = −0.18 e Å−3 |
2832 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 1132 Fridel pairs |
141 parameters | Absolute structure parameter: 0.012 (9) |
0 restraints |
Experimental. SADABS |
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 | ||
Cu | 0.151860 (16) | 0.151860 (16) | 0.0000 | 0.01397 (9) | |
S | −0.01348 (3) | 0.16903 (4) | 0.067367 (18) | 0.01868 (10) | |
C1 | −0.08987 (14) | 0.29169 (14) | 0.02823 (7) | 0.0139 (3) | |
C2 | −0.27499 (14) | 0.44307 (15) | 0.01431 (7) | 0.0193 (3) | |
H2A | −0.2115 | 0.4959 | −0.0086 | 0.023* | |
H2B | −0.3180 | 0.5009 | 0.0437 | 0.023* | |
C3 | −0.37665 (16) | 0.38819 (17) | −0.02821 (8) | 0.0244 (3) | |
H3A | −0.4209 | 0.4599 | −0.0488 | 0.037* | |
H3B | −0.4405 | 0.3373 | −0.0055 | 0.037* | |
H3C | −0.3341 | 0.3320 | −0.0578 | 0.037* | |
C4 | −0.27172 (15) | 0.28546 (16) | 0.09915 (7) | 0.0199 (3) | |
H4A | −0.2523 | 0.1912 | 0.1024 | 0.024* | |
H4B | −0.3670 | 0.2953 | 0.0941 | 0.024* | |
C5 | −0.23001 (17) | 0.35315 (19) | 0.15659 (8) | 0.0293 (4) | |
H5A | −0.2765 | 0.3147 | 0.1906 | 0.044* | |
H5B | −0.2507 | 0.4462 | 0.1540 | 0.044* | |
H5C | −0.1360 | 0.3421 | 0.1622 | 0.044* | |
C6 | 0.12967 (13) | 0.35602 (13) | −0.08980 (7) | 0.0140 (3) | |
C7 | 0.05412 (15) | 0.41548 (14) | −0.13431 (7) | 0.0179 (3) | |
H7 | −0.0371 | 0.4257 | −0.1290 | 0.022* | |
C8 | 0.11421 (15) | 0.45922 (15) | −0.18616 (7) | 0.0215 (3) | |
H8 | 0.0631 | 0.4980 | −0.2168 | 0.026* | |
C9 | 0.24836 (16) | 0.44715 (14) | −0.19406 (7) | 0.0206 (3) | |
H9 | 0.2882 | 0.4780 | −0.2297 | 0.025* | |
C10 | 0.32348 (15) | 0.38972 (14) | −0.14959 (7) | 0.0180 (3) | |
H10 | 0.4150 | 0.3818 | −0.1546 | 0.022* | |
C11 | 0.26463 (14) | 0.34395 (14) | −0.09783 (7) | 0.0157 (3) | |
H11 | 0.3161 | 0.3041 | −0.0676 | 0.019* | |
N1 | 0.07845 (11) | 0.30528 (11) | −0.03596 (6) | 0.0128 (2) | |
N2 | −0.04083 (11) | 0.34544 (12) | −0.02319 (5) | 0.0142 (2) | |
N3 | −0.20557 (12) | 0.33844 (12) | 0.04624 (6) | 0.0162 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu | 0.01257 (10) | 0.01257 (10) | 0.01677 (15) | 0.00385 (8) | −0.00076 (6) | 0.00076 (6) |
S | 0.01651 (17) | 0.02061 (19) | 0.0189 (2) | 0.00520 (13) | 0.00276 (14) | 0.00644 (14) |
C1 | 0.0132 (6) | 0.0147 (6) | 0.0140 (7) | 0.0002 (5) | −0.0012 (5) | −0.0015 (5) |
C2 | 0.0161 (7) | 0.0176 (7) | 0.0243 (8) | 0.0069 (5) | 0.0016 (6) | 0.0014 (6) |
C3 | 0.0250 (8) | 0.0267 (8) | 0.0216 (8) | 0.0102 (6) | −0.0030 (6) | −0.0019 (6) |
C4 | 0.0151 (7) | 0.0250 (8) | 0.0195 (8) | 0.0017 (6) | 0.0039 (6) | 0.0010 (6) |
C5 | 0.0271 (8) | 0.0413 (10) | 0.0196 (8) | −0.0002 (7) | 0.0014 (7) | −0.0027 (8) |
C6 | 0.0150 (6) | 0.0121 (6) | 0.0147 (6) | 0.0011 (5) | −0.0002 (5) | −0.0016 (5) |
C7 | 0.0156 (6) | 0.0174 (7) | 0.0208 (8) | 0.0039 (5) | −0.0013 (6) | 0.0004 (6) |
C8 | 0.0260 (8) | 0.0211 (7) | 0.0175 (8) | 0.0041 (6) | −0.0017 (6) | 0.0027 (6) |
C9 | 0.0293 (8) | 0.0154 (7) | 0.0171 (7) | −0.0004 (6) | 0.0055 (6) | −0.0015 (6) |
C10 | 0.0173 (7) | 0.0149 (6) | 0.0219 (8) | −0.0009 (5) | 0.0029 (6) | −0.0050 (6) |
C11 | 0.0149 (6) | 0.0146 (6) | 0.0177 (7) | 0.0011 (5) | 0.0001 (5) | −0.0017 (6) |
N1 | 0.0107 (5) | 0.0122 (5) | 0.0156 (6) | 0.0013 (4) | −0.0001 (5) | −0.0016 (5) |
N2 | 0.0126 (5) | 0.0138 (5) | 0.0161 (6) | 0.0017 (5) | 0.0000 (4) | −0.0006 (5) |
N3 | 0.0133 (5) | 0.0178 (6) | 0.0175 (6) | 0.0032 (5) | 0.0026 (5) | 0.0017 (5) |
Cu—N1i | 1.9219 (12) | C4—H4B | 0.9900 |
Cu—N1 | 1.9219 (12) | C5—H5A | 0.9800 |
Cu—Si | 2.2756 (4) | C5—H5B | 0.9800 |
Cu—S | 2.2756 (4) | C5—H5C | 0.9800 |
S—C1 | 1.7220 (15) | C6—C7 | 1.401 (2) |
C1—N3 | 1.3427 (18) | C6—C11 | 1.4024 (19) |
C1—N2 | 1.3706 (18) | C6—N1 | 1.4128 (19) |
C2—N3 | 1.4733 (18) | C7—C8 | 1.387 (2) |
C2—C3 | 1.520 (2) | C7—H7 | 0.9500 |
C2—H2A | 0.9900 | C8—C9 | 1.394 (2) |
C2—H2B | 0.9900 | C8—H8 | 0.9500 |
C3—H3A | 0.9800 | C9—C10 | 1.389 (2) |
C3—H3B | 0.9800 | C9—H9 | 0.9500 |
C3—H3C | 0.9800 | C10—C11 | 1.387 (2) |
C4—N3 | 1.4682 (19) | C10—H10 | 0.9500 |
C4—C5 | 1.521 (2) | C11—H11 | 0.9500 |
C4—H4A | 0.9900 | N1—N2 | 1.3230 (16) |
N1i—Cu—N1 | 144.83 (7) | H5A—C5—H5B | 109.5 |
N1i—Cu—Si | 85.46 (4) | C4—C5—H5C | 109.5 |
N1—Cu—Si | 111.39 (4) | H5A—C5—H5C | 109.5 |
N1i—Cu—S | 111.39 (4) | H5B—C5—H5C | 109.5 |
N1—Cu—S | 85.46 (4) | C7—C6—C11 | 119.62 (14) |
Si—Cu—S | 123.60 (2) | C7—C6—N1 | 124.01 (12) |
C1—S—Cu | 93.44 (5) | C11—C6—N1 | 116.36 (13) |
N3—C1—N2 | 115.62 (12) | C8—C7—C6 | 119.20 (13) |
N3—C1—S | 120.77 (11) | C8—C7—H7 | 120.4 |
N2—C1—S | 123.58 (10) | C6—C7—H7 | 120.4 |
N3—C2—C3 | 111.40 (13) | C7—C8—C9 | 121.08 (14) |
N3—C2—H2A | 109.3 | C7—C8—H8 | 119.5 |
C3—C2—H2A | 109.3 | C9—C8—H8 | 119.5 |
N3—C2—H2B | 109.3 | C10—C9—C8 | 119.70 (15) |
C3—C2—H2B | 109.3 | C10—C9—H9 | 120.2 |
H2A—C2—H2B | 108.0 | C8—C9—H9 | 120.2 |
C2—C3—H3A | 109.5 | C11—C10—C9 | 119.92 (14) |
C2—C3—H3B | 109.5 | C11—C10—H10 | 120.0 |
H3A—C3—H3B | 109.5 | C9—C10—H10 | 120.0 |
C2—C3—H3C | 109.5 | C10—C11—C6 | 120.46 (14) |
H3A—C3—H3C | 109.5 | C10—C11—H11 | 119.8 |
H3B—C3—H3C | 109.5 | C6—C11—H11 | 119.8 |
N3—C4—C5 | 112.36 (13) | N2—N1—C6 | 114.41 (11) |
N3—C4—H4A | 109.1 | N2—N1—Cu | 121.86 (9) |
C5—C4—H4A | 109.1 | C6—N1—Cu | 120.82 (9) |
N3—C4—H4B | 109.1 | N1—N2—C1 | 113.29 (12) |
C5—C4—H4B | 109.1 | C1—N3—C4 | 121.22 (12) |
H4A—C4—H4B | 107.9 | C1—N3—C2 | 122.89 (12) |
C4—C5—H5A | 109.5 | C4—N3—C2 | 115.88 (11) |
C4—C5—H5B | 109.5 |
Symmetry code: (i) y, x, −z. |
C22H30N6PdS2 | F(000) = 1128 |
Mr = 549.04 | Dx = 1.508 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 16.0360 (16) Å | Cell parameters from 2763 reflections |
b = 12.4564 (13) Å | θ = 2.5–27.8° |
c = 12.3311 (12) Å | µ = 0.96 mm−1 |
β = 100.952 (2)° | T = 118 K |
V = 2418.3 (4) Å3 | Plate, green |
Z = 4 | 0.30 × 0.25 × 0.01 mm |
CCD area detector diffractometer | 2847 independent reflections |
Radiation source: fine-focus sealed tube | 2431 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
Detector resolution: 8.192 pixels mm-1 | θmax = 28.0°, θmin = 2.1° |
ω scans | h = −19→21 |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | k = −16→16 |
Tmin = 0.761, Tmax = 0.990 | l = −9→16 |
8430 measured reflections |
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)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0337P)2 + 16.6377P] where P = (Fo2 + 2Fc2)/3 |
2847 reflections | (Δ/σ)max < 0.001 |
191 parameters | Δρmax = 1.47 e Å−3 |
0 restraints | Δρmin = −2.28 e Å−3 |
C22H30N6PdS2 | V = 2418.3 (4) Å3 |
Mr = 549.04 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 16.0360 (16) Å | µ = 0.96 mm−1 |
b = 12.4564 (13) Å | T = 118 K |
c = 12.3311 (12) Å | 0.30 × 0.25 × 0.01 mm |
β = 100.952 (2)° |
CCD area detector diffractometer | 2847 independent reflections |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | 2431 reflections with I > 2σ(I) |
Tmin = 0.761, Tmax = 0.990 | Rint = 0.043 |
8430 measured reflections |
R[F2 > 2σ(F2)] = 0.049 | 0 restraints |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0337P)2 + 16.6377P] where P = (Fo2 + 2Fc2)/3 |
2847 reflections | Δρmax = 1.47 e Å−3 |
191 parameters | Δρmin = −2.28 e Å−3 |
Experimental. SADABS |
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 | ||
Pd | 0.2500 | 0.2500 | 0.0000 | 0.00766 (12) | |
S | 0.20585 (6) | 0.09864 (8) | −0.10047 (9) | 0.0124 (2) | |
N1 | 0.3590 (2) | 0.2174 (3) | −0.0483 (3) | 0.0105 (7) | |
N2 | 0.3672 (2) | 0.1407 (3) | −0.1216 (3) | 0.0130 (7) | |
N3 | 0.3036 (2) | −0.0007 (3) | −0.2235 (3) | 0.0166 (8) | |
C1 | 0.2987 (2) | 0.0782 (3) | −0.1514 (3) | 0.0133 (8) | |
C2 | 0.2362 (3) | −0.0810 (3) | −0.2519 (4) | 0.0181 (9) | |
H2A | 0.2348 | −0.1059 | −0.3268 | 0.022* | |
H2B | 0.1819 | −0.0479 | −0.2494 | 0.022* | |
C3 | 0.2491 (3) | −0.1763 (4) | −0.1742 (4) | 0.0267 (11) | |
H3A | 0.2037 | −0.2268 | −0.1956 | 0.040* | |
H3B | 0.2495 | −0.1523 | −0.1001 | 0.040* | |
H3C | 0.3023 | −0.2102 | −0.1775 | 0.040* | |
C4 | 0.3812 (3) | −0.0184 (4) | −0.2689 (4) | 0.0223 (10) | |
H4A | 0.3859 | −0.0940 | −0.2854 | 0.027* | |
H4B | 0.4304 | 0.0014 | −0.2138 | 0.027* | |
C5 | 0.3810 (3) | 0.0463 (4) | −0.3727 (4) | 0.0310 (12) | |
H5A | 0.4325 | 0.0327 | −0.3995 | 0.046* | |
H5B | 0.3774 | 0.1213 | −0.3566 | 0.046* | |
H5C | 0.3331 | 0.0259 | −0.4281 | 0.046* | |
C6 | 0.4352 (2) | 0.2783 (3) | −0.0210 (3) | 0.0119 (8) | |
C7 | 0.4701 (2) | 0.3000 (3) | 0.0893 (3) | 0.0133 (8) | |
H7 | 0.4440 | 0.2741 | 0.1453 | 0.016* | |
C8 | 0.5442 (3) | 0.3608 (3) | 0.1151 (4) | 0.0166 (9) | |
H8 | 0.5675 | 0.3756 | 0.1886 | 0.020* | |
C9 | 0.5835 (3) | 0.3992 (3) | 0.0325 (4) | 0.0198 (9) | |
H9 | 0.6330 | 0.4394 | 0.0502 | 0.024* | |
C10 | 0.5486 (3) | 0.3774 (3) | −0.0775 (4) | 0.0185 (9) | |
H10 | 0.5745 | 0.4041 | −0.1333 | 0.022* | |
C11 | 0.4749 (3) | 0.3156 (3) | −0.1045 (4) | 0.0148 (8) | |
H11 | 0.4525 | 0.2995 | −0.1779 | 0.018* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd | 0.00897 (19) | 0.00730 (18) | 0.0072 (2) | −0.00099 (16) | 0.00277 (14) | −0.00066 (17) |
S | 0.0122 (4) | 0.0116 (4) | 0.0139 (5) | −0.0023 (4) | 0.0042 (4) | −0.0043 (4) |
N1 | 0.0113 (15) | 0.0103 (14) | 0.0109 (17) | −0.0001 (12) | 0.0041 (13) | −0.0014 (12) |
N2 | 0.0140 (16) | 0.0126 (15) | 0.0131 (18) | 0.0014 (12) | 0.0043 (13) | −0.0014 (13) |
N3 | 0.0166 (17) | 0.0146 (17) | 0.020 (2) | −0.0006 (13) | 0.0072 (15) | −0.0078 (15) |
C1 | 0.0140 (18) | 0.0126 (18) | 0.014 (2) | 0.0013 (14) | 0.0033 (16) | −0.0006 (15) |
C2 | 0.018 (2) | 0.018 (2) | 0.019 (2) | −0.0026 (16) | 0.0047 (17) | −0.0100 (17) |
C3 | 0.030 (2) | 0.017 (2) | 0.034 (3) | −0.0007 (18) | 0.007 (2) | −0.006 (2) |
C4 | 0.017 (2) | 0.026 (2) | 0.027 (3) | 0.0016 (17) | 0.0103 (19) | −0.013 (2) |
C5 | 0.026 (2) | 0.042 (3) | 0.027 (3) | −0.005 (2) | 0.011 (2) | −0.008 (2) |
C6 | 0.0139 (18) | 0.0079 (17) | 0.014 (2) | 0.0016 (13) | 0.0038 (16) | −0.0008 (14) |
C7 | 0.0159 (19) | 0.0139 (18) | 0.012 (2) | 0.0009 (15) | 0.0066 (16) | 0.0028 (16) |
C8 | 0.017 (2) | 0.019 (2) | 0.013 (2) | −0.0020 (16) | −0.0019 (17) | −0.0029 (16) |
C9 | 0.017 (2) | 0.017 (2) | 0.026 (3) | −0.0064 (16) | 0.0046 (18) | −0.0021 (18) |
C10 | 0.018 (2) | 0.018 (2) | 0.022 (2) | −0.0045 (16) | 0.0100 (18) | −0.0005 (18) |
C11 | 0.018 (2) | 0.0145 (19) | 0.013 (2) | −0.0024 (15) | 0.0045 (16) | −0.0020 (16) |
Pd—N1i | 1.993 (3) | C4—C5 | 1.512 (7) |
Pd—N1 | 1.993 (3) | C4—H4A | 0.9700 |
Pd—S | 2.2930 (10) | C4—H4B | 0.9700 |
Pd—Si | 2.2930 (10) | C5—H5A | 0.9600 |
S—C1 | 1.741 (4) | C5—H5B | 0.9600 |
N1—N2 | 1.339 (5) | C5—H5C | 0.9600 |
N1—C6 | 1.423 (5) | C6—C11 | 1.389 (6) |
N2—C1 | 1.340 (5) | C6—C7 | 1.396 (6) |
N3—C1 | 1.338 (5) | C7—C8 | 1.395 (6) |
N3—C2 | 1.465 (5) | C7—H7 | 0.9300 |
N3—C4 | 1.476 (5) | C8—C9 | 1.381 (6) |
C2—C3 | 1.515 (6) | C8—H8 | 0.9300 |
C2—H2A | 0.9700 | C9—C10 | 1.392 (6) |
C2—H2B | 0.9700 | C9—H9 | 0.9300 |
C3—H3A | 0.9600 | C10—C11 | 1.397 (6) |
C3—H3B | 0.9600 | C10—H10 | 0.9300 |
C3—H3C | 0.9600 | C11—H11 | 0.9300 |
N1i—Pd—N1 | 180.0 | N3—C4—H4A | 109.2 |
N1i—Pd—S | 97.51 (9) | C5—C4—H4A | 109.2 |
N1—Pd—S | 82.49 (9) | N3—C4—H4B | 109.2 |
N1i—Pd—Si | 82.49 (9) | C5—C4—H4B | 109.2 |
N1—Pd—Si | 97.51 (9) | H4A—C4—H4B | 107.9 |
S—Pd—Si | 180.00 (5) | C4—C5—H5A | 109.5 |
C1—S—Pd | 96.75 (14) | C4—C5—H5B | 109.5 |
N2—N1—C6 | 110.5 (3) | H5A—C5—H5B | 109.5 |
N2—N1—Pd | 123.5 (2) | C4—C5—H5C | 109.5 |
C6—N1—Pd | 125.7 (3) | H5A—C5—H5C | 109.5 |
N1—N2—C1 | 114.8 (3) | H5B—C5—H5C | 109.5 |
C1—N3—C2 | 121.8 (4) | C11—C6—C7 | 120.2 (4) |
C1—N3—C4 | 121.5 (3) | C11—C6—N1 | 119.8 (4) |
C2—N3—C4 | 116.4 (3) | C7—C6—N1 | 120.1 (4) |
N3—C1—N2 | 117.4 (4) | C8—C7—C6 | 119.6 (4) |
N3—C1—S | 120.6 (3) | C8—C7—H7 | 120.2 |
N2—C1—S | 122.0 (3) | C6—C7—H7 | 120.2 |
N3—C2—C3 | 112.2 (4) | C9—C8—C7 | 120.5 (4) |
N3—C2—H2A | 109.2 | C9—C8—H8 | 119.7 |
C3—C2—H2A | 109.2 | C7—C8—H8 | 119.7 |
N3—C2—H2B | 109.2 | C8—C9—C10 | 119.8 (4) |
C3—C2—H2B | 109.2 | C8—C9—H9 | 120.1 |
H2A—C2—H2B | 107.9 | C10—C9—H9 | 120.1 |
C2—C3—H3A | 109.5 | C9—C10—C11 | 120.3 (4) |
C2—C3—H3B | 109.5 | C9—C10—H10 | 119.9 |
H3A—C3—H3B | 109.5 | C11—C10—H10 | 119.9 |
C2—C3—H3C | 109.5 | C6—C11—C10 | 119.6 (4) |
H3A—C3—H3C | 109.5 | C6—C11—H11 | 120.2 |
H3B—C3—H3C | 109.5 | C10—C11—H11 | 120.2 |
N3—C4—C5 | 112.1 (4) |
Symmetry code: (i) −x+1/2, −y+1/2, −z. |
C22H30N6PtS2 | F(000) = 1256 |
Mr = 637.73 | Dx = 1.745 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 15.9317 (7) Å | Cell parameters from 9821 reflections |
b = 12.5300 (5) Å | θ = 2.5–28.0° |
c = 12.3798 (5) Å | µ = 5.97 mm−1 |
β = 100.755 (1)° | T = 118 K |
V = 2427.90 (17) Å3 | Plate, dark green |
Z = 4 | 0.25 × 0.20 × 0.15 mm |
CCD area detector diffractometer | 2937 independent reflections |
Radiation source: fine-focus sealed tube | 2632 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.120 |
Detector resolution: 8.192 pixels mm-1 | θmax = 28.0°, θmin = 2.1° |
ω scans | h = −21→21 |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | k = −16→16 |
Tmin = 0.255, Tmax = 0.408 | l = −16→16 |
14253 measured reflections |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0604P)2] where P = (Fo2 + 2Fc2)/3 |
2937 reflections | (Δ/σ)max < 0.001 |
144 parameters | Δρmax = 3.08 e Å−3 |
0 restraints | Δρmin = −4.14 e Å−3 |
C22H30N6PtS2 | V = 2427.90 (17) Å3 |
Mr = 637.73 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 15.9317 (7) Å | µ = 5.97 mm−1 |
b = 12.5300 (5) Å | T = 118 K |
c = 12.3798 (5) Å | 0.25 × 0.20 × 0.15 mm |
β = 100.755 (1)° |
CCD area detector diffractometer | 2937 independent reflections |
Absorption correction: empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | 2632 reflections with I > 2σ(I) |
Tmin = 0.255, Tmax = 0.408 | Rint = 0.120 |
14253 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.098 | H-atom parameters constrained |
S = 1.09 | Δρmax = 3.08 e Å−3 |
2937 reflections | Δρmin = −4.14 e Å−3 |
144 parameters |
Experimental. SADABS |
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 | ||
Pt1 | 0.2500 | 0.2500 | 0.5000 | 0.01078 (10) | |
S1 | 0.20567 (4) | 0.09968 (5) | 0.39979 (5) | 0.01557 (15) | |
N1 | 0.35741 (13) | 0.2183 (2) | 0.45030 (17) | 0.0132 (4) | |
N2 | 0.36679 (13) | 0.14186 (17) | 0.37671 (16) | 0.0161 (4) | |
N3 | 0.30312 (14) | 0.00106 (18) | 0.27523 (17) | 0.0219 (5) | |
C1 | 0.29868 (15) | 0.08026 (19) | 0.34732 (19) | 0.0164 (5) | |
C2 | 0.23519 (17) | −0.0786 (2) | 0.2480 (2) | 0.0230 (5) | |
H2A | 0.2332 | −0.1033 | 0.1732 | 0.028* | |
H2B | 0.1807 | −0.0456 | 0.2514 | 0.028* | |
C3 | 0.2486 (2) | −0.1735 (2) | 0.3253 (3) | 0.0314 (6) | |
H3A | 0.3031 | −0.2055 | 0.3233 | 0.047* | |
H3B | 0.2042 | −0.2249 | 0.3027 | 0.047* | |
H3C | 0.2472 | −0.1501 | 0.3987 | 0.047* | |
C4 | 0.38099 (17) | −0.0158 (2) | 0.2293 (2) | 0.0270 (6) | |
H4A | 0.3861 | −0.0911 | 0.2131 | 0.032* | |
H4B | 0.4305 | 0.0043 | 0.2837 | 0.032* | |
C5 | 0.38013 (19) | 0.0485 (3) | 0.1252 (2) | 0.0381 (7) | |
H5A | 0.3276 | 0.0358 | 0.0747 | 0.057* | |
H5B | 0.4274 | 0.0273 | 0.0919 | 0.057* | |
H5C | 0.3849 | 0.1231 | 0.1430 | 0.057* | |
C6 | 0.43498 (17) | 0.2789 (3) | 0.4786 (2) | 0.0153 (5) | |
C7 | 0.47029 (16) | 0.2975 (2) | 0.58875 (19) | 0.0178 (5) | |
H7 | 0.4440 | 0.2705 | 0.6440 | 0.021* | |
C8 | 0.54517 (16) | 0.3568 (2) | 0.6154 (2) | 0.0204 (5) | |
H8 | 0.5691 | 0.3688 | 0.6888 | 0.025* | |
C9 | 0.58436 (16) | 0.3981 (2) | 0.5334 (2) | 0.0225 (5) | |
H9 | 0.6339 | 0.4386 | 0.5514 | 0.027* | |
C10 | 0.54854 (17) | 0.3783 (2) | 0.4236 (2) | 0.0222 (5) | |
H10 | 0.5746 | 0.4058 | 0.3683 | 0.027* | |
C11 | 0.47520 (16) | 0.3185 (2) | 0.39599 (19) | 0.0193 (5) | |
H11 | 0.4525 | 0.3045 | 0.3226 | 0.023* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.01491 (14) | 0.00946 (15) | 0.00856 (15) | −0.00097 (3) | 0.00371 (9) | −0.00063 (3) |
S1 | 0.0192 (3) | 0.0136 (3) | 0.0150 (3) | −0.0025 (2) | 0.0058 (2) | −0.0044 (2) |
N1 | 0.0152 (11) | 0.0119 (10) | 0.0132 (11) | −0.0016 (10) | 0.0042 (8) | −0.0002 (10) |
N2 | 0.0202 (10) | 0.0158 (10) | 0.0132 (9) | 0.0009 (8) | 0.0051 (8) | −0.0035 (8) |
N3 | 0.0237 (11) | 0.0210 (11) | 0.0227 (11) | −0.0027 (9) | 0.0088 (9) | −0.0097 (9) |
C1 | 0.0216 (11) | 0.0151 (12) | 0.0139 (11) | 0.0022 (9) | 0.0067 (9) | −0.0005 (9) |
C2 | 0.0266 (13) | 0.0212 (13) | 0.0211 (13) | −0.0022 (11) | 0.0041 (10) | −0.0104 (10) |
C3 | 0.0376 (16) | 0.0213 (14) | 0.0353 (16) | −0.0019 (12) | 0.0064 (13) | −0.0048 (12) |
C4 | 0.0248 (13) | 0.0286 (15) | 0.0297 (15) | 0.0013 (11) | 0.0104 (11) | −0.0141 (11) |
C5 | 0.0330 (16) | 0.052 (2) | 0.0322 (16) | −0.0060 (15) | 0.0139 (13) | −0.0101 (15) |
C6 | 0.0150 (13) | 0.0126 (11) | 0.0180 (13) | −0.0004 (12) | 0.0025 (10) | −0.0022 (12) |
C7 | 0.0234 (12) | 0.0178 (13) | 0.0131 (11) | 0.0006 (10) | 0.0058 (9) | 0.0011 (9) |
C8 | 0.0229 (12) | 0.0206 (13) | 0.0165 (12) | −0.0008 (10) | 0.0003 (9) | −0.0015 (10) |
C9 | 0.0192 (11) | 0.0225 (13) | 0.0263 (13) | −0.0054 (10) | 0.0053 (10) | −0.0022 (10) |
C10 | 0.0257 (12) | 0.0228 (13) | 0.0210 (13) | −0.0045 (10) | 0.0120 (10) | 0.0003 (10) |
C11 | 0.0243 (12) | 0.0213 (12) | 0.0129 (11) | −0.0015 (10) | 0.0051 (9) | −0.0011 (9) |
Pt1—N1i | 1.964 (2) | C4—C5 | 1.518 (4) |
Pt1—N1 | 1.964 (2) | C4—H4A | 0.9700 |
Pt1—S1 | 2.2932 (6) | C4—H4B | 0.9700 |
Pt1—S1i | 2.2932 (6) | C5—H5A | 0.9600 |
S1—C1 | 1.743 (2) | C5—H5B | 0.9600 |
N1—N2 | 1.349 (3) | C5—H5C | 0.9600 |
N1—C6 | 1.437 (4) | C6—C7 | 1.394 (4) |
N2—C1 | 1.326 (3) | C6—C11 | 1.395 (4) |
N3—C1 | 1.345 (3) | C7—C8 | 1.392 (4) |
N3—C2 | 1.465 (3) | C7—H7 | 0.9300 |
N3—C4 | 1.474 (3) | C8—C9 | 1.387 (3) |
C2—C3 | 1.516 (4) | C8—H8 | 0.9300 |
C2—H2A | 0.9700 | C9—C10 | 1.395 (4) |
C2—H2B | 0.9700 | C9—H9 | 0.9300 |
C3—H3A | 0.9600 | C10—C11 | 1.376 (4) |
C3—H3B | 0.9600 | C10—H10 | 0.9300 |
C3—H3C | 0.9600 | C11—H11 | 0.9300 |
N1i—Pt1—N1 | 180.0 | N3—C4—H4A | 109.2 |
N1i—Pt1—S1 | 97.89 (7) | C5—C4—H4A | 109.2 |
N1—Pt1—S1 | 82.11 (7) | N3—C4—H4B | 109.2 |
N1i—Pt1—S1i | 82.11 (7) | C5—C4—H4B | 109.2 |
N1—Pt1—S1i | 97.89 (7) | H4A—C4—H4B | 107.9 |
S1—Pt1—S1i | 180.000 (17) | C4—C5—H5A | 109.5 |
C1—S1—Pt1 | 96.82 (8) | C4—C5—H5B | 109.5 |
N2—N1—C6 | 109.9 (2) | H5A—C5—H5B | 109.5 |
N2—N1—Pt1 | 124.60 (17) | C4—C5—H5C | 109.5 |
C6—N1—Pt1 | 125.2 (2) | H5A—C5—H5C | 109.5 |
C1—N2—N1 | 114.23 (19) | H5B—C5—H5C | 109.5 |
C1—N3—C2 | 121.9 (2) | C7—C6—C11 | 120.0 (3) |
C1—N3—C4 | 121.0 (2) | C7—C6—N1 | 119.9 (2) |
C2—N3—C4 | 116.9 (2) | C11—C6—N1 | 120.1 (2) |
N2—C1—N3 | 118.0 (2) | C8—C7—C6 | 119.5 (2) |
N2—C1—S1 | 121.71 (18) | C8—C7—H7 | 120.2 |
N3—C1—S1 | 120.26 (19) | C6—C7—H7 | 120.2 |
N3—C2—C3 | 112.2 (2) | C9—C8—C7 | 120.6 (2) |
N3—C2—H2A | 109.2 | C9—C8—H8 | 119.7 |
C3—C2—H2A | 109.2 | C7—C8—H8 | 119.7 |
N3—C2—H2B | 109.2 | C8—C9—C10 | 119.2 (2) |
C3—C2—H2B | 109.2 | C8—C9—H9 | 120.4 |
H2A—C2—H2B | 107.9 | C10—C9—H9 | 120.4 |
C2—C3—H3A | 109.5 | C11—C10—C9 | 120.9 (2) |
C2—C3—H3B | 109.5 | C11—C10—H10 | 119.6 |
H3A—C3—H3B | 109.5 | C9—C10—H10 | 119.6 |
C2—C3—H3C | 109.5 | C10—C11—C6 | 119.8 (2) |
H3A—C3—H3C | 109.5 | C10—C11—H11 | 120.1 |
H3B—C3—H3C | 109.5 | C6—C11—H11 | 120.1 |
N3—C4—C5 | 112.1 (2) | ||
N1i—Pt1—S1—C1 | 175.13 (10) | C1—N3—C2—C3 | −88.5 (3) |
N1—Pt1—S1—C1 | −4.87 (10) | C4—N3—C2—C3 | 85.2 (3) |
S1—Pt1—N1—N2 | 7.3 (2) | C1—N3—C4—C5 | −88.9 (3) |
S1i—Pt1—N1—N2 | −172.7 (2) | C2—N3—C4—C5 | 97.4 (3) |
S1—Pt1—N1—C6 | −178.8 (2) | N2—N1—C6—C7 | −130.9 (3) |
S1i—Pt1—N1—C6 | 1.2 (2) | Pt1—N1—C6—C7 | 54.5 (4) |
C6—N1—N2—C1 | 178.7 (2) | N2—N1—C6—C11 | 48.7 (4) |
Pt1—N1—N2—C1 | −6.6 (3) | Pt1—N1—C6—C11 | −125.9 (2) |
N1—N2—C1—N3 | −179.1 (2) | C11—C6—C7—C8 | 0.8 (4) |
N1—N2—C1—S1 | 0.7 (3) | N1—C6—C7—C8 | −179.6 (3) |
C2—N3—C1—N2 | 172.6 (2) | C6—C7—C8—C9 | 0.6 (4) |
C4—N3—C1—N2 | −0.8 (4) | C7—C8—C9—C10 | −0.9 (4) |
C2—N3—C1—S1 | −7.2 (3) | C8—C9—C10—C11 | 0.0 (4) |
C4—N3—C1—S1 | 179.4 (2) | C9—C10—C11—C6 | 1.3 (4) |
Pt1—S1—C1—N2 | 3.8 (2) | C7—C6—C11—C10 | −1.7 (4) |
Pt1—S1—C1—N3 | −176.34 (19) | N1—C6—C11—C10 | 178.7 (3) |
Symmetry code: (i) −x+1/2, −y+1/2, −z+1. |
Experimental details
(NiL20) | (CuL20) | (PdL20) | (PtL20) | |
Crystal data | ||||
Chemical formula | C22H30N6NiS2 | C22H30CuN6S2 | C22H30N6PdS2 | C22H30N6PtS2 |
Mr | 501.35 | 506.18 | 549.04 | 637.73 |
Crystal system, space group | Tetragonal, P41212 | Tetragonal, P41212 | Monoclinic, C2/c | Monoclinic, C2/c |
Temperature (K) | 118 | 118 | 118 | 118 |
a, b, c (Å) | 10.2852 (3), 10.2852 (3), 22.2862 (13) | 10.2643 (4), 10.2643 (4), 22.3519 (13) | 16.0360 (16), 12.4564 (13), 12.3311 (12) | 15.9317 (7), 12.5300 (5), 12.3798 (5) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 100.952 (2), 90 | 90, 100.755 (1), 90 |
V (Å3) | 2357.55 (17) | 2354.90 (19) | 2418.3 (4) | 2427.90 (17) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 1.02 | 1.13 | 0.96 | 5.97 |
Crystal size (mm) | 0.50 × 0.30 × 0.05 | 0.40 × 0.35 × 0.15 | 0.30 × 0.25 × 0.01 | 0.25 × 0.20 × 0.15 |
Data collection | ||||
Diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer | CCD area detector diffractometer |
Absorption correction | Empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | Empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | Empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) | Empirical (using intensity measurements) SADABS,ver2.03 (Sheldrick,2001) |
Tmin, Tmax | 0.74, 0.96 | 0.661, 0.849 | 0.761, 0.990 | 0.255, 0.408 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 31608, 3630, 3436 | 16807, 2832, 2788 | 8430, 2847, 2431 | 14253, 2937, 2632 |
Rint | 0.043 | 0.027 | 0.043 | 0.120 |
(sin θ/λ)max (Å−1) | 0.725 | 0.661 | 0.661 | 0.660 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.078, 1.16 | 0.024, 0.070, 1.10 | 0.049, 0.105, 1.13 | 0.037, 0.098, 1.09 |
No. of reflections | 3630 | 2832 | 2847 | 2937 |
No. of parameters | 201 | 141 | 191 | 144 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0407P)2 + 0.3442P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.P)2 + 0.1079P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0337P)2 + 16.6377P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0604P)2] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.61, −0.26 | 0.36, −0.18 | 1.47, −2.28 | 3.08, −4.14 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881, 1132 Fridel pairs | ? | ? |
Absolute structure parameter | 0.021 (12) | 0.012 (9) | ? | ? |
Computer programs: Bruker SMART (Bruker AXS,1998), Bruker SMART, Bruker SHELXTL (Sheldrick,2001), Bruker SHELXTL, WinGX publication routines (Farrugia, 1999).
Cu—N1i | 1.9219 (12) | C1—N2 | 1.3706 (18) |
Cu—Si | 2.2756 (4) | N1—N2 | 1.3230 (16) |
S—C1 | 1.7220 (15) | ||
N1i—Cu—N1 | 144.83 (7) | Si—Cu—S | 123.60 (2) |
N1i—Cu—Si | 85.46 (4) |
Symmetry code: (i) y, x, −z. |
Pt1—N1i | 1.964 (2) | N1—N2 | 1.349 (3) |
Pt1—S1 | 2.2932 (6) | N2—C1 | 1.326 (3) |
S1—C1 | 1.743 (2) | ||
N1i—Pt1—N1 | 180.0 | S1—Pt1—S1i | 180.000 (17) |
N1—Pt1—S1 | 82.11 (7) |
Symmetry code: (i) −x+1/2, −y+1/2, −z+1. |
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