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The title cationic complex μ-guanidinido-bis­[(2,2′:6′,2′′-ter­pyridine)­platinum(II)], [Pt2(C15H11N3)2(CH4N3)]3+, has a twofold axis and shows a stacked dinuclear structure with a short Pt...Pt distance of 3.0749 (6) Å. The complexes are further stacked to form a columnar structure in the crystal of the title compound.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802007468/ob6125sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802007468/ob6125Isup2.hkl
Contains datablock I

CCDC reference: 189283

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.020 Å
  • R factor = 0.058
  • wR factor = 0.174
  • Data-to-parameter ratio = 13.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 3 PLAT_321 Alert C Check Hybridisation of C(17) in solvent/ion ? PLAT_420 Alert C D-H Without Acceptor N(5) - H(14) ? PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 26 N2 -PT1 -N4 -C16 0.00 5.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 42 N4 -PT1 -N2 -C6 -115.00 5.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 43 N4 -PT1 -N2 -C10 61.00 5.00 1.555 1.555 1.555 1.555 PLAT_733 Alert C Torsion Calc 22.9(9), Rep 23.0(3) .... 3.00 s.u-Ratio PT1 -N4 -C16 -N4 1.555 1.555 1.555 2.655 General Notes
ABSTM_02 The ratio of expected to reported Tmax/Tmin(RR) is > 2.00 Tmin and Tmax reported: 0.418 0.999 Tmin and Tmax expected: 0.033 0.603 RR = 7.713 Please check that your absorption correction is appropriate.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
7 Alert Level C = Please check

Computing details top

Data collection: Rigaku/AFC Diffractometer Control Software (Rigaku, 1995); cell refinement: Rigaku/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation and Rigaku, 2000)'; program(s) used to solve structure: SIR92 (Altomare, 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
[Pt2(C15H11N3)2(CH4N3)](PF6)3·2C2H3NDx = 2.087 Mg m3
Mr = 1431.78Mo Kα radiation, λ = 0.7107 Å
Monoclinic, C2/cCell parameters from 24 reflections
a = 17.000 (5) Åθ = 14.9–15.0°
b = 20.351 (4) ŵ = 6.33 mm1
c = 13.915 (4) ÅT = 296 K
β = 108.87 (2)°Plate, red
V = 4555 (1) Å30.60 × 0.50 × 0.08 mm
Z = 4
Data collection top
Rigaku AFC-7R
diffractometer
Rint = 0.038
ω–2θ scansθmax = 27.5°
Absorption correction: analytical
(de Meulenaer & Tompa, 1965)
h = 222
Tmin = 0.418, Tmax = 0.999k = 026
6172 measured reflectionsl = 1817
5243 independent reflections3 standard reflections every 150 reflections
3897 reflections with I > 2σ(I) intensity decay: 5.6%
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.058 w = 1/[σ2(Fo2) + (0.136P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.174(Δ/σ)max = 0.002
S = 1.02Δρmax = 2.69 e Å3
3897 reflectionsΔρmin = 3.42 e Å3
299 parameters
Special details top

Refinement. Refinement using reflections with F2 > -10.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt10.48419 (2)0.06339 (1)0.13479 (2)0.0399 (2)
P10.7835 (3)0.2342 (2)0.2103 (3)0.091 (1)
P21.00000.0412 (2)0.25000.071 (1)
F10.6909 (7)0.2086 (5)0.176 (1)0.155 (5)
F20.7532 (8)0.3033 (5)0.1600 (8)0.128 (4)
F30.776 (1)0.2615 (6)0.3122 (9)0.174 (6)
F40.7932 (8)0.2064 (6)0.1089 (9)0.141 (4)
F50.8147 (8)0.1649 (5)0.2631 (9)0.137 (4)
F60.8751 (7)0.2603 (5)0.2401 (8)0.139 (4)
F70.9311 (5)0.0123 (5)0.2082 (9)0.127 (4)
F80.9317 (5)0.0975 (5)0.2126 (9)0.128 (4)
F91.017 (1)0.0421 (9)0.1469 (10)0.162 (5)
N10.5979 (4)0.0215 (3)0.1689 (5)0.041 (1)
N20.4485 (5)0.0255 (4)0.0991 (5)0.044 (1)
N30.3600 (6)0.0771 (5)0.0832 (6)0.059 (2)
N40.5181 (5)0.1552 (3)0.1769 (6)0.049 (2)
N50.50000.2546 (5)0.25000.084 (5)
N60.978 (1)0.2192 (8)0.519 (1)0.12180 (6)*
C10.6723 (6)0.0505 (5)0.2018 (7)0.052 (2)
C20.7445 (6)0.0148 (6)0.2239 (9)0.066 (3)
C30.7406 (7)0.0527 (6)0.2133 (9)0.069 (3)
C40.6653 (7)0.0835 (5)0.1799 (8)0.059 (2)
C50.5942 (6)0.0453 (4)0.1554 (6)0.043 (2)
C60.5095 (6)0.0725 (4)0.1172 (6)0.045 (2)
C70.4839 (8)0.1380 (5)0.0952 (9)0.067 (3)
C80.4001 (8)0.1530 (6)0.0582 (8)0.074 (3)
C90.3412 (7)0.1036 (6)0.0422 (8)0.067 (3)
C100.3661 (6)0.0392 (6)0.0625 (7)0.057 (2)
C110.3159 (6)0.0206 (7)0.0529 (7)0.063 (3)
C120.2295 (8)0.0203 (9)0.015 (1)0.096 (5)
C130.1898 (8)0.079 (1)0.009 (1)0.123 (7)
C140.234 (1)0.136 (1)0.039 (1)0.113 (6)
C150.3192 (7)0.1350 (6)0.0753 (8)0.074 (3)
C160.50000.1885 (6)0.25000.055 (3)
C171.004 (1)0.1799 (9)0.479 (1)0.10480 (6)*
C181.021 (2)0.133 (2)0.411 (3)0.2022 (2)*
H20.67420.09830.20950.0519*
H30.79750.03680.24610.0665*
H40.79090.07860.22840.0689*
H50.66040.13160.17260.0589*
H60.52550.17320.10580.0667*
H70.38270.19840.04380.0738*
H80.28220.11470.01850.0672*
H90.19790.02080.00420.0956*
H100.13010.08270.01650.1234*
H110.20410.17760.03140.1127*
H120.35120.17680.09550.0742*
H130.54870.17530.14590.0486*
H140.45680.27580.25380.0841*
H160.98820.09480.40620.2022*
H171.01810.14990.34920.2022*
H181.08050.11710.44410.2022*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.0503 (2)0.0392 (2)0.0321 (2)0.0001 (1)0.0162 (1)0.0005 (1)
P10.113 (3)0.077 (2)0.089 (2)0.050 (2)0.039 (2)0.014 (2)
P20.048 (2)0.077 (3)0.082 (3)0.00000.011 (2)0.0000
F10.123 (8)0.104 (7)0.26 (2)0.052 (6)0.084 (9)0.007 (8)
F20.164 (9)0.096 (6)0.122 (8)0.046 (6)0.043 (7)0.010 (5)
F30.31 (2)0.136 (9)0.120 (8)0.03 (1)0.13 (1)0.000 (7)
F40.162 (10)0.154 (9)0.105 (7)0.044 (8)0.039 (7)0.054 (7)
F50.167 (10)0.092 (6)0.147 (9)0.039 (6)0.043 (8)0.002 (6)
F60.126 (7)0.138 (8)0.136 (8)0.077 (7)0.019 (6)0.010 (7)
F70.077 (5)0.114 (7)0.18 (1)0.014 (5)0.033 (6)0.036 (7)
F80.080 (5)0.113 (7)0.166 (9)0.024 (5)0.004 (6)0.000 (7)
F90.20 (1)0.19 (1)0.124 (9)0.01 (1)0.088 (9)0.009 (9)
N10.048 (3)0.042 (3)0.033 (3)0.006 (3)0.014 (3)0.001 (3)
N20.053 (4)0.050 (4)0.029 (3)0.002 (3)0.013 (3)0.000 (3)
N30.061 (5)0.080 (6)0.034 (4)0.016 (4)0.014 (3)0.003 (4)
N40.069 (4)0.033 (3)0.051 (4)0.002 (3)0.029 (4)0.009 (3)
N50.13 (1)0.024 (5)0.12 (1)0.00000.06 (1)0.0000
C10.053 (5)0.058 (5)0.048 (5)0.015 (4)0.021 (4)0.008 (4)
C20.047 (5)0.095 (9)0.061 (6)0.014 (5)0.021 (4)0.002 (6)
C30.059 (6)0.088 (8)0.061 (6)0.019 (5)0.020 (5)0.008 (5)
C40.071 (6)0.055 (5)0.051 (5)0.014 (5)0.021 (5)0.007 (4)
C50.057 (5)0.037 (4)0.037 (4)0.002 (3)0.018 (3)0.002 (3)
C60.064 (5)0.043 (4)0.037 (4)0.003 (4)0.027 (4)0.003 (3)
C70.100 (8)0.045 (5)0.066 (6)0.012 (5)0.043 (6)0.001 (5)
C80.104 (9)0.060 (6)0.059 (6)0.043 (6)0.028 (6)0.016 (5)
C90.071 (6)0.084 (8)0.053 (5)0.038 (6)0.028 (5)0.015 (5)
C100.061 (5)0.075 (6)0.037 (4)0.027 (5)0.019 (4)0.014 (4)
C110.049 (5)0.102 (9)0.039 (4)0.006 (5)0.015 (4)0.019 (5)
C120.051 (6)0.17 (2)0.065 (7)0.001 (8)0.018 (5)0.024 (9)
C130.049 (6)0.23 (2)0.069 (9)0.04 (1)0.004 (6)0.03 (1)
C140.088 (9)0.17 (2)0.063 (8)0.06 (1)0.006 (7)0.021 (9)
C150.075 (7)0.087 (8)0.057 (6)0.035 (6)0.016 (5)0.005 (5)
C160.081 (8)0.042 (6)0.049 (6)0.00000.031 (6)0.0000
Geometric parameters (Å, º) top
Pt1—N12.024 (7)C1—H20.978
Pt1—N21.922 (7)C2—C31.38 (2)
Pt1—N32.018 (9)C2—H30.963
Pt1—N41.987 (7)C3—C41.37 (2)
P1—F11.58 (1)C3—H40.968
P1—F21.58 (1)C4—C51.39 (1)
P1—F31.57 (1)C4—H50.984
P1—F41.58 (1)C5—C61.47 (1)
P1—F51.60 (1)C6—C71.40 (1)
P1—F61.57 (1)C7—C81.38 (2)
P2—F71.567 (10)C7—H60.984
P2—F7i1.567 (10)C8—C91.38 (2)
P2—F81.593 (10)C8—H70.972
P2—F8i1.593 (10)C9—C101.38 (2)
P2—F91.55 (2)C9—H80.977
P2—F9i1.55 (2)C10—C111.47 (2)
N1—C11.34 (1)C11—C121.39 (2)
N1—C51.37 (1)C12—C131.37 (3)
N2—C61.37 (1)C12—H90.985
N2—C101.36 (1)C13—C141.36 (3)
N3—C111.36 (2)C13—H100.963
N3—C151.35 (2)C14—C151.37 (2)
N4—C161.34 (1)C14—H110.982
N4—H130.877C15—H121.001
N5—C161.35 (2)C17—C181.43 (5)
N5—H140.868C18—H160.952
N5—H14ii0.868C18—H170.913
N6—C171.14 (3)C18—H181.015
C1—C21.37 (1)
Pt1···Pt1ii3.0749 (6)F7···C13iii3.58 (2)
Pt1···C6iii3.548 (10)F8···C13iii3.12 (2)
F1···C8iii3.32 (2)F8···N5vii3.21 (1)
F2···C9iv3.18 (2)F9···C13iii3.56 (2)
F2···C4v3.19 (1)N1···C10iii3.49 (1)
F2···C8iv3.36 (2)N1···N2iii3.553 (9)
F2···C3v3.40 (2)N3···C4iii3.55 (1)
F2···F4vi3.57 (2)N4···N6viii3.30 (2)
F3···C4v3.30 (2)N5···N6ix3.16 (2)
F4···C9iii3.30 (2)N5···N6viii3.16 (2)
F4···F4vi3.41 (2)N6···C7v3.47 (2)
F4···C8iii3.53 (2)C1···C9iii3.50 (2)
F4···C8iv3.58 (2)C1···C10iii3.53 (1)
F6···C8iv3.22 (2)C2···C12iii3.57 (2)
F6···C7v3.42 (1)C3···C12iii3.44 (2)
F6···C4v3.51 (2)C3···C11iii3.57 (2)
F7···C12iii3.47 (2)C4···C11iii3.59 (2)
N1—Pt1—N282.0 (3)C2—C1—H2120.5
N1—Pt1—N3162.1 (3)C1—C2—C3119.6 (10)
N1—Pt1—N499.4 (3)C1—C2—H3120.0
N2—Pt1—N380.3 (3)C3—C2—H3120.4
N2—Pt1—N4177.1 (4)C2—C3—C4120 (1)
N3—Pt1—N498.4 (4)C2—C3—H4120.7
F1—P1—F290.6 (6)C4—C3—H4119.1
F1—P1—F391.3 (9)C3—C4—C5118 (1)
F1—P1—F489.7 (8)C3—C4—H5122.2
F1—P1—F589.9 (6)C5—C4—H5119.7
F1—P1—F6177.8 (8)N1—C5—C4121.7 (8)
F2—P1—F388.6 (7)N1—C5—C6114.9 (7)
F2—P1—F492.1 (7)C4—C5—C6123.4 (8)
F2—P1—F5179.0 (6)N2—C6—C5113.3 (7)
F2—P1—F688.2 (6)N2—C6—C7117.3 (9)
F3—P1—F4178.8 (8)C5—C6—C7129.4 (9)
F3—P1—F590.5 (7)C6—C7—C8119 (1)
F3—P1—F690.4 (8)C6—C7—H6120.0
F4—P1—F588.8 (7)C8—C7—H6120.0
F4—P1—F688.5 (7)C7—C8—C9120 (1)
F5—P1—F691.3 (6)C7—C8—H7119.6
F7—P2—F7i91.9 (7)C9—C8—H7120.2
F7—P2—F890.0 (5)C8—C9—C10119 (1)
F7—P2—F8i177.3 (6)C8—C9—H8119.8
F7—P2—F990.3 (8)C10—C9—H8120.2
F7—P2—F9i90.6 (8)N2—C10—C9118.9 (10)
F7i—P2—F8177.3 (6)N2—C10—C11111.3 (9)
F7i—P2—F8i90.0 (5)C9—C10—C11129.8 (10)
F7i—P2—F990.6 (8)N3—C11—C10115.2 (9)
F7i—P2—F9i90.3 (8)N3—C11—C12121 (1)
F8—P2—F8i88.1 (7)C10—C11—C12122 (1)
F8—P2—F991.4 (8)C11—C12—C13117 (1)
F8—P2—F9i87.7 (8)C11—C12—H9121.5
F8i—P2—F987.7 (8)C13—C12—H9121.0
F8i—P2—F9i91.4 (8)C12—C13—C14120 (1)
F9—P2—F9i178 (1)C12—C13—H10121.7
PT1—N1—C1128.3 (6)C14—C13—H10117.6
PT1—N1—C5112.7 (5)C13—C14—C15121 (1)
C1—N1—C5118.9 (8)C13—C14—H11119.3
PT1—N2—C6116.9 (6)C15—C14—H11119.5
PT1—N2—C10119.5 (7)N3—C15—C14119 (1)
C6—N2—C10123.6 (8)N3—C15—H12120.1
PT1—N3—C11113.6 (7)C14—C15—H12120.6
PT1—N3—C15126.7 (8)N4—C16—N4ii119 (1)
C11—N3—C15119.6 (9)N4—C16—N5120.5 (6)
PT1—N4—C16125.8 (7)N4ii—C16—N5120.5 (6)
PT1—N4—H13117.1N6—C17—C18168 (1)
C16—N4—H13117.1C17—C18—H16110.6
C16—N5—H14119.8C17—C18—H17114.2
C16—N5—H14ii119.8C17—C18—H18107.7
H14—N5—H14ii120.4H16—C18—H17112.5
N1—C1—C2121.4 (9)H16—C18—H18104.1
N1—C1—H2118.1H17—C18—H18107.0
PT1—N1—C1—C2178.5 (8)N3—PT1—N2—C101.9 (7)
PT1—N1—C5—C4176.4 (8)N3—PT1—N4—C1663.6 (6)
PT1—N1—C5—C61.3 (9)N3—C11—C10—C9177 (1)
PT1—N2—C6—C54 (1)N3—C11—C12—C130 (1)
PT1—N2—C6—C7177.5 (8)N3—C15—C14—C131 (2)
PT1—N2—C10—C9176.7 (8)N4—PT1—N1—C15.0 (8)
PT1—N2—C10—C112 (1)N4—PT1—N1—C5174.7 (6)
PT1—N3—C11—C100 (1)N4—PT1—N2—C6115 (5)
PT1—N3—C11—C12180.0 (9)N4—PT1—N2—C1061 (5)
PT1—N3—C15—C14179.6 (10)N4—PT1—N3—C11176.2 (7)
PT1—N4—C16—N4ii23.0 (3)N4—PT1—N3—C154.8 (10)
PT1—N4—C16—N5157.0 (3)C1—N1—C5—C43 (1)
N1—PT1—N2—C63.8 (6)C1—N1—C5—C6179.0 (8)
N1—PT1—N2—C10179.3 (7)C1—C2—C3—C40 (1)
N1—PT1—N3—C119 (1)C2—C1—N1—C51 (1)
N1—PT1—N3—C15169.5 (9)C2—C3—C4—C51 (1)
N1—PT1—N4—C16118.1 (6)C3—C4—C5—C6179 (1)
N1—C1—C2—C30 (1)C4—C5—C6—C72 (1)
N1—C5—C4—C33 (1)C5—C6—N2—C10179.2 (8)
N1—C5—C6—N21 (1)C5—C6—C7—C8179 (1)
N1—C5—C6—C7179 (1)C6—N2—C10—C90 (1)
N2—PT1—N1—C1177.6 (8)C6—N2—C10—C11178.8 (8)
N2—PT1—N1—C52.7 (6)C6—C7—C8—C90 (1)
N2—PT1—N3—C111.2 (7)C7—C6—N2—C100 (1)
N2—PT1—N3—C15177.8 (10)C7—C8—C9—C100 (1)
N2—PT1—N4—C160 (5)C8—C9—C10—C11179 (1)
N2—C6—C5—C4179.3 (9)C9—C10—C11—C122 (1)
N2—C6—C7—C80 (1)C10—C11—N3—C15178.7 (10)
N2—C10—C9—C80 (1)C10—C11—C12—C13179 (1)
N2—C10—C11—N31 (1)C11—N3—C15—C141 (1)
N2—C10—C11—C12178 (1)C11—C12—C13—C140 (2)
N3—PT1—N1—C1169 (1)C12—C11—N3—C150 (1)
N3—PT1—N1—C511 (1)C12—C13—C14—C151 (2)
N3—PT1—N2—C6178.8 (7)C12—C13—C14—C151 (2)
Symmetry codes: (i) x+2, y, z+1/2; (ii) x+1, y, z+1/2; (iii) x+1, y, z; (iv) x+1/2, y+1/2, z; (v) x+3/2, y+1/2, z+1/2; (vi) x+3/2, y+1/2, z; (vii) x+1/2, y1/2, z; (viii) x1/2, y+1/2, z1/2; (ix) x+3/2, y+1/2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H13···F10.882.413.14 (1)140
N5—H14···N6ix0.873.003.16 (2)93
N5—H14···F8x0.872.653.21 (1)123
Symmetry codes: (ix) x+3/2, y+1/2, z+1; (x) x1/2, y+1/2, z.
 

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