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In the title compound, [Pt2(C7H8N2O)2(NH3)4](ClO4)4, the head-to-head isomer of the PtII dimer has a mirror plane through the Pt—Pt bond axis. The intradimer Pt—Pt distance is 3.0569 (8) Å, while the shortest interdimer Pt...Pt distance is 7.2325 (9) Å. Two adjacent dimers are associated with one another, with a π-stacking interaction between the N-methyl­pyridinium moieties, where the plane-to-plane separation is 3.27 (1) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803014521/ob6266sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803014521/ob6266Isup2.hkl
Contains datablock I

CCDC reference: 221615

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.013 Å
  • Disorder in solvent or counterion
  • R factor = 0.035
  • wR factor = 0.062
  • Data-to-parameter ratio = 10.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
THETM_01 Alert B The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5554
Yellow Alert Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.116 PLAT_302 Alert C Anion/Solvent Disorder ......................... 17.00 Perc.
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check

Computing details top

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: KENX (Sakai, 2002); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEPII (Johnson, 1976).

bis(µ-N-methylisonicotinamidato)bis[cis-diammineplatinum(II)] tetraperchlorate top
Crystal data top
[Pt2(C7H8N2O)2(NH3)4](ClO4)4F(000) = 2144
Mr = 1128.42Dx = 2.416 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2336 reflections
a = 17.9590 (7) Åθ = 2.3–22.0°
b = 17.0728 (7) ŵ = 9.44 mm1
c = 10.1189 (4) ÅT = 296 K
V = 3102.6 (2) Å3Prism, pale green
Z = 40.06 × 0.05 × 0.03 mm
Data collection top
Bruker SMART APEX CCD-detector
diffractometer
2317 independent reflections
Radiation source: fine-focus sealed tube1576 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.117
Detector resolution: 8.366 pixels mm-1θmax = 23.3°, θmin = 2.3°
ω scansh = 1919
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1818
Tmin = 0.540, Tmax = 0.753l = 118
16797 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.062H-atom parameters constrained
S = 0.88 w = 1/[σ2(Fo2) + (0.0194P)2]
where P = (Fo2 + 2Fc2)/3
2317 reflections(Δ/σ)max = 0.001
221 parametersΔρmax = 1.43 e Å3
0 restraintsΔρmin = 0.66 e Å3
Special details top

Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data.

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.

Mean-plane data from final SHELXL refinement run:-

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

2.2104 (0.0689) x - 0.0000 (0.0000) y + 10.0420 (0.0048) z = 7.5908 (0.0136)

* 0.0000 (0.0000) N1 * 0.0000 (0.0000) N3 * 0.0000 (0.0000) N1_$2 * 0.0000 (0.0000) N3_$2 0.0666 (0.0053) Pt1 2.8762 (0.0071) Pt2

Rms deviation of fitted atoms = 0.0000

- 9.1575 (0.0541) x + 0.0000 (0.0002) y + 8.7046 (0.0181) z = 7.0753 (0.0279)

Angle to previous plane (with approximate e.s.d.) = 37.73 (0.23)

* 0.0000 (0.0000) O1 * 0.0000 (0.0000) N2 * 0.0000 (0.0000) O1_$2 * 0.0000 (0.0000) N2_$2 - 3.0082 (0.0052) Pt1 - 0.0489 (0.0048) Pt2

Rms deviation of fitted atoms = 0.0000

12.1367 (0.2207) x - 11.9206 (0.2258) y + 2.3898 (0.0576) z = 1.6468 (0.1032)

Angle to previous plane (with approximate e.s.d.) = 81.87 (0.48)

* 0.0000 (0.0000) O1 * 0.0000 (0.0000) C1 * 0.0000 (0.0000) N3

Rms deviation of fitted atoms = 0.0000

8.9020 (0.0587) x - 8.0276 (0.0551) y + 7.3889 (0.0285) z = 5.7518 (0.0220)

Angle to previous plane (with approximate e.s.d.) = 33.31 (0.91)

* 0.0150 (0.0066) C2 * -0.0100 (0.0071) C3 * 0.0001 (0.0072) C4 * 0.0005 (0.0066) C5 * -0.0104 (0.0067) C6 * 0.0049 (0.0065) N4

Rms deviation of fitted atoms = 0.0087

2.2031 (0.0689) x - 0.7756 (0.0613) y + 10.0319 (0.0051) z = 7.4546 (0.0208)

Angle to previous plane (with approximate e.s.d.) = 36.28 (1/3)

* 0.0000 (0.0000) N1 * 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) N3

Rms deviation of fitted atoms = 0.0000

- 9.1594 (0.0541) x + 0.5871 (0.0572) y + 8.6969 (0.0183) z = 7.1652 (0.0295)

Angle to previous plane (with approximate e.s.d.) = 38.00 (0.23)

* 0.0000 (0.0000) N2 * 0.0000 (0.0000) Pt2 * 0.0000 (0.0000) O1

Rms deviation of fitted atoms = 0.0000

12.1367 (0.2207) x - 11.9206 (0.2258) y + 2.3898 (0.0576) z = 1.6468 (0.1032)

Angle to previous plane (with approximate e.s.d.) = 80.46 (1/2)

* 0.0000 (0.0000) O1 * 0.0000 (0.0000) C1 * 0.0000 (0.0000) N3

Rms deviation of fitted atoms = 0.0000

8.9020 (0.0587) x - 8.0276 (0.0551) y + 7.3889 (0.0285) z = 5.7518 (0.0220)

Angle to previous plane (with approximate e.s.d.) = 33.31 (0.91)

* 0.0150 (0.0066) C2 * -0.0100 (0.0071) C3 * 0.0001 (0.0072) C4 * 0.0005 (0.0066) C5 * -0.0104 (0.0067) C6 * 0.0049 (0.0065) N4

Rms deviation of fitted atoms = 0.0087

12.1367 (0.2207) x - 11.9206 (0.2258) y + 2.3898 (0.0576) z = 1.6468 (0.1032)

Angle to previous plane (with approximate e.s.d.) = 33.31 (0.91)

* 0.0000 (0.0000) O1 * 0.0000 (0.0000) C1 * 0.0000 (0.0000) N3

Rms deviation of fitted atoms = 0.0000

2.2031 (0.0689) x - 0.7756 (0.0613) y + 10.0319 (0.0051) z = 7.4546 (0.0208)

Angle to previous plane (with approximate e.s.d.) = 69.59 (0.42)

* 0.0000 (0.0000) N1 * 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) N3

Rms deviation of fitted atoms = 0.0000

8.9020 (0.0587) x - 8.0276 (0.0551) y + 7.3889 (0.0285) z = 5.7518 (0.0220)

Angle to previous plane (with approximate e.s.d.) = 36.28 (1/3)

* 0.0150 (0.0066) C2 * -0.0100 (0.0071) C3 * 0.0001 (0.0072) C4 * 0.0005 (0.0066) C5 * -0.0104 (0.0067) C6 * 0.0049 (0.0065) N4 3.2593 (0.0165) C2_$4 3.2843 (0.0170) C3_$4 3.2743 (0.0165) C4_$4 3.2739 (0.0166) C5_$4 3.2848 (0.0165) C6_$4 3.2694 (0.0167) N4_$4

Rms deviation of fitted atoms = 0.0087

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt10.23213 (3)0.25000.71144 (6)0.03159 (17)
Pt20.18482 (3)0.25001.00164 (6)0.03133 (16)
Cl10.23659 (17)0.02242 (15)0.4016 (3)0.0449 (7)
Cl20.3939 (3)0.25000.3650 (5)0.0643 (13)
Cl30.4567 (2)0.25000.9050 (4)0.0437 (10)
O10.1145 (3)0.1655 (4)0.9333 (7)0.0468 (19)
O20.2474 (4)0.0326 (5)0.2665 (7)0.086 (3)
O30.1775 (4)0.0338 (4)0.4210 (8)0.076 (2)
O40.2140 (4)0.0932 (4)0.4580 (8)0.086 (3)
O50.3029 (4)0.0059 (4)0.4624 (7)0.072 (3)
O60.4070 (9)0.25000.2335 (14)0.129 (5)
O70.3148 (12)0.25000.365 (2)0.193 (9)
O80.4091 (7)0.1827 (7)0.4249 (11)0.189 (6)
O90.4660 (5)0.25000.7644 (9)0.054 (3)
O10A0.4133 (6)0.1802 (6)0.9417 (10)0.072 (3)*0.740 (9)
O10B0.4988 (16)0.1797 (18)0.952 (3)0.072 (3)*0.260 (9)
O11A0.5245 (8)0.25000.9767 (15)0.072 (3)*0.740 (9)
O11B0.376 (2)0.25000.942 (4)0.072 (3)*0.260 (17)
N10.3103 (4)0.1637 (4)0.6876 (8)0.047 (2)
H40.32040.15800.60210.071*
H20.29270.11880.71970.071*
H30.35160.17680.73070.071*
N20.2534 (4)0.1679 (4)1.0794 (8)0.041 (2)
H60.25330.17181.16710.062*
H70.29940.17531.04930.062*
H50.23770.12041.05600.062*
N30.1554 (4)0.1647 (4)0.7217 (7)0.032 (2)
H10.14970.13950.64890.039*
N40.0258 (4)0.0557 (4)0.7497 (9)0.037 (2)
C10.1138 (5)0.1408 (5)0.8136 (10)0.032 (3)
C20.0614 (5)0.0740 (5)0.7868 (9)0.029 (2)
C30.0809 (5)0.0164 (6)0.6974 (10)0.042 (3)
H80.12410.02140.64750.050*
C40.0364 (5)0.0477 (6)0.6827 (11)0.049 (3)
H90.05040.08680.62380.058*
C50.0474 (5)0.0013 (6)0.8343 (10)0.041 (3)
H100.09160.00760.88110.049*
C60.0047 (5)0.0649 (6)0.8532 (10)0.036 (3)
H110.02070.10370.91120.043*
C70.0708 (5)0.1290 (5)0.7344 (11)0.064 (4)
H140.06580.16050.81250.096*
H120.05320.15790.65920.096*
H130.12220.11560.72190.096*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.0360 (3)0.0274 (3)0.0314 (3)0.0000.0042 (3)0.000
Pt20.0367 (3)0.0287 (3)0.0286 (3)0.0000.0001 (3)0.000
Cl10.0616 (19)0.0376 (16)0.0356 (16)0.0049 (16)0.0014 (17)0.0004 (13)
Cl20.095 (4)0.064 (3)0.034 (3)0.0000.013 (3)0.000
Cl30.043 (2)0.051 (3)0.037 (2)0.0000.003 (2)0.000
O10.043 (4)0.061 (5)0.036 (4)0.012 (4)0.001 (4)0.005 (4)
O20.114 (7)0.113 (7)0.031 (5)0.038 (5)0.016 (5)0.024 (4)
O30.080 (6)0.072 (6)0.077 (6)0.028 (5)0.004 (5)0.001 (5)
O40.102 (7)0.048 (5)0.107 (8)0.010 (5)0.002 (6)0.040 (5)
O50.067 (6)0.084 (6)0.065 (6)0.014 (5)0.013 (5)0.015 (5)
O60.184 (15)0.139 (13)0.065 (11)0.0000.003 (11)0.000
O70.189 (19)0.178 (19)0.21 (2)0.0000.043 (18)0.000
O80.283 (15)0.145 (11)0.140 (10)0.057 (11)0.018 (11)0.101 (9)
O90.069 (7)0.075 (7)0.017 (6)0.0000.009 (5)0.000
N10.052 (5)0.033 (5)0.056 (6)0.001 (4)0.002 (5)0.002 (4)
N20.044 (6)0.037 (5)0.043 (5)0.006 (4)0.005 (5)0.003 (4)
N30.040 (5)0.034 (5)0.023 (5)0.008 (4)0.004 (4)0.007 (4)
N40.032 (5)0.029 (5)0.051 (7)0.001 (4)0.006 (5)0.008 (5)
C10.035 (6)0.028 (6)0.033 (7)0.004 (5)0.003 (6)0.000 (5)
C20.028 (6)0.029 (6)0.029 (6)0.001 (5)0.007 (6)0.005 (5)
C30.031 (6)0.042 (6)0.053 (7)0.006 (5)0.013 (6)0.011 (6)
C40.036 (7)0.048 (7)0.062 (9)0.005 (6)0.012 (7)0.023 (6)
C50.026 (7)0.042 (7)0.055 (8)0.003 (6)0.005 (6)0.001 (6)
C60.036 (6)0.032 (6)0.040 (7)0.009 (5)0.009 (6)0.013 (6)
C70.050 (7)0.040 (7)0.102 (11)0.023 (6)0.006 (7)0.001 (7)
Geometric parameters (Å, º) top
Pt1—N32.007 (7)Cl2—O61.351 (13)
Pt1—N12.049 (7)Cl2—O71.420 (19)
Pt1—Pt23.0569 (8)Cl3—O11A1.417 (15)
Pt2—N22.025 (6)Cl3—O91.432 (9)
Pt2—O12.038 (6)Cl3—O10A1.472 (10)
Pt1—Pt2i7.2325 (9)Cl3—O11B1.50 (4)
O1—C11.282 (10)Cl3—O10B1.50 (3)
N3—C11.260 (10)N1—H40.8900
N4—C41.313 (11)N1—H20.8900
N4—C51.322 (11)N1—H30.8900
N4—C71.498 (10)N2—H60.8900
C1—C21.505 (11)N2—H70.8900
C2—C61.372 (11)N2—H50.8900
C2—C31.381 (12)N3—H10.8600
C3—C41.364 (12)C3—H80.9300
C5—C61.380 (12)C4—H90.9300
Cl1—O21.392 (7)C5—H100.9300
Cl1—O41.397 (7)C6—H110.9300
Cl1—O51.424 (7)C7—H140.9600
Cl1—O31.444 (7)C7—H120.9600
Cl2—O81.327 (9)C7—H130.9600
N3—Pt1—N3ii93.0 (4)O11A—Cl3—O9114.2 (8)
N3—Pt1—N1ii176.2 (3)O11A—Cl3—O10A109.1 (6)
N3—Pt1—N187.4 (3)O9—Cl3—O10A108.2 (5)
N1ii—Pt1—N191.9 (4)O10A—Cl3—O10Aii108.0 (8)
N3—Pt1—Pt276.1 (2)O9—Cl3—O11B111.3 (17)
N1—Pt1—Pt2107.7 (2)O9—Cl3—O10B105.0 (12)
N2ii—Pt2—N287.6 (4)O11B—Cl3—O10B114.1 (13)
N2ii—Pt2—O1177.0 (3)O10Bii—Cl3—O10B107 (2)
N2—Pt2—O191.1 (3)Pt1—N1—H4109.5
O1—Pt2—O1ii90.1 (4)Pt1—N1—H2109.5
N2—Pt2—Pt1101.8 (2)H4—N1—H2109.5
O1—Pt2—Pt181.15 (18)Pt1—N1—H3109.5
C1—O1—Pt2124.0 (6)H4—N1—H3109.5
C1—N3—Pt1132.8 (7)H2—N1—H3109.5
C4—N4—C5120.8 (8)Pt2—N2—H6109.5
C4—N4—C7119.5 (8)Pt2—N2—H7109.5
C5—N4—C7119.7 (8)H6—N2—H7109.5
N3—C1—O1125.8 (9)Pt2—N2—H5109.5
N3—C1—C2118.9 (9)H6—N2—H5109.5
O1—C1—C2115.2 (9)H7—N2—H5109.5
C6—C2—C3117.4 (8)C1—N3—H1113.6
C6—C2—C1122.6 (9)Pt1—N3—H1113.6
C3—C2—C1120.0 (8)C4—C3—H8120.2
C4—C3—C2119.6 (9)C2—C3—H8120.2
N4—C4—C3121.7 (9)N4—C4—H9119.2
N4—C5—C6120.1 (9)C3—C4—H9119.2
C2—C6—C5120.4 (9)N4—C5—H10119.9
O2—Cl1—O4109.5 (5)C6—C5—H10119.9
O2—Cl1—O5110.5 (5)C2—C6—H11119.8
O4—Cl1—O5111.1 (5)C5—C6—H11119.8
O2—Cl1—O3108.6 (5)N4—C7—H14109.5
O4—Cl1—O3107.9 (5)N4—C7—H12109.5
O5—Cl1—O3109.2 (5)H14—C7—H12109.5
O8—Cl2—O8ii119.9 (12)N4—C7—H13109.5
O8—Cl2—O6114.4 (6)H14—C7—H13109.5
O8—Cl2—O7101.9 (8)H12—C7—H13109.5
O6—Cl2—O7100.0 (11)
N1—Pt1—Pt2—N24.0 (3)C5—N4—C4—C30.0 (16)
N3—Pt1—Pt2—O12.6 (3)C7—N4—C4—C3177.2 (9)
N3—C1—C2—C6151.7 (9)C2—C3—C4—N41.4 (16)
O1—C1—C2—C632.1 (13)C4—N4—C5—C60.1 (15)
N3—C1—C2—C331.8 (13)C7—N4—C5—C6177.2 (9)
O1—C1—C2—C3144.4 (9)C3—C2—C6—C52.9 (14)
C6—C2—C3—C42.8 (15)C1—C2—C6—C5173.8 (8)
C1—C2—C3—C4173.9 (9)N4—C5—C6—C21.5 (15)
Symmetry codes: (i) x, y, z1; (ii) x, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H4···O40.892.653.136 (11)116
N1—H4···O80.892.433.213 (13)146
N1—H3···O10A0.892.413.180 (12)146
N3—H1···O40.862.383.118 (11)143
N2—H5···O3iii0.892.523.058 (11)119
N2—H6···O2iv0.892.582.988 (10)109
N2—H5···O5iii0.892.293.174 (10)171
N2—H7···O11Bii0.892.172.96 (4)148
Symmetry codes: (ii) x, y+1/2, z; (iii) x+1/2, y, z+1/2; (iv) x, y, z+1.
 

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