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In the crystal, the cations and anions form a layered structure via strong N—H...Cl, weak C—H...Cl and C—H...O hydrogen bonds and π-stacking inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989023005157/zv2027sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989023005157/zv2027Isup2.hkl
Contains datablock I

CCDC reference: 2268577

Key indicators

Structure: I
  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.022
  • wR factor = 0.041
  • Data-to-parameter ratio = 20.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ Please Check PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min). 6 Note PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L= 0.600 3 Report
Alert level G PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 2 Note PLAT019_ALERT_1_G _diffrn_measured_fraction_theta_full/*_max < 1.0 0.998 Report PLAT164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct. 1 Note PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 1 Report PLAT480_ALERT_4_G Long H...A H-Bond Reported H5C ..CL2 . 2.91 Ang. PLAT794_ALERT_5_G Tentative Bond Valency for Pt1 (II) . 2.91 Info PLAT802_ALERT_4_G CIF Input Record(s) with more than 80 Characters 1 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 1 Note PLAT933_ALERT_2_G Number of HKL-OMIT Records in Embedded .res File 1 Note PLAT941_ALERT_3_G Average HKL Measurement Multiplicity ........... 2.7 Low PLAT967_ALERT_5_G Note: Two-Theta Cutoff Value in Embedded .res .. 60.0 Degree PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 1 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 3 ALERT level C = Check. Ensure it is not caused by an omission or oversight 12 ALERT level G = General information/check it is not something unexpected 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX3 (Bruker, 2018); cell refinement: SAINT v7.68A (Bruker, 2013); data reduction: SAINT v7.68A (Bruker, 2013); program(s) used to solve structure: SHELXT2018/2 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: Olex2 1.5 (Dolomanov et al., 2009); software used to prepare material for publication: Olex2 1.5 (Dolomanov et al., 2009).

Bis(1,3,7-trimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-9-ium) hexachloridoplatinum(IV) top
Crystal data top
(C8H11N4O2)2[PtCl6]Z = 1
Mr = 798.20F(000) = 386
Triclinic, P1Dx = 2.135 Mg m3
a = 7.8800 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.1542 (2) ÅCell parameters from 4212 reflections
c = 10.5374 (3) Åθ = 3.1–29.8°
α = 95.784 (2)°µ = 6.34 mm1
β = 91.525 (2)°T = 296 K
γ = 112.472 (1)°Plate, orange
V = 620.92 (3) Å30.18 × 0.08 × 0.02 mm
Data collection top
Bruker Kappa APEXII area-detector
diffractometer
3573 reflections with I > 2σ(I)
φ and ω scansRint = 0.035
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
θmax = 30.0°, θmin = 3.5°
Tmin = 0.734, Tmax = 1.000h = 1111
9764 measured reflectionsk = 1111
3616 independent reflectionsl = 1414
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.022H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.041 w = 1/[σ2(Fo2) + (0.0171P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
3616 reflectionsΔρmax = 0.45 e Å3
173 parametersΔρmin = 0.89 e Å3
1 restraint
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt10.0000000.0000000.0000000.02050 (4)
Cl10.04784 (10)0.01026 (9)0.21599 (5)0.03560 (15)
Cl20.30304 (9)0.03978 (10)0.04685 (6)0.03557 (14)
Cl30.08989 (10)0.30803 (8)0.01376 (6)0.03532 (14)
O10.5394 (3)0.1187 (3)0.3683 (2)0.0474 (5)
O20.1510 (3)0.4010 (3)0.4685 (2)0.0517 (6)
N10.5642 (3)0.6187 (3)0.1713 (2)0.0340 (5)
H10.656 (3)0.646 (4)0.126 (3)0.053 (10)*
N20.3378 (3)0.6487 (3)0.2696 (2)0.0317 (5)
N30.5758 (3)0.3628 (3)0.2700 (2)0.0296 (5)
N40.3502 (3)0.2641 (3)0.42037 (19)0.0289 (5)
C10.3648 (4)0.5055 (3)0.3126 (2)0.0271 (5)
C20.5073 (4)0.4880 (3)0.2510 (2)0.0269 (5)
C30.4589 (4)0.7135 (4)0.1859 (3)0.0378 (7)
H30.475 (4)0.812 (4)0.150 (3)0.046 (9)*
C40.1984 (5)0.7171 (4)0.3115 (3)0.0485 (8)
H4A0.1272410.6459100.3732530.058*0.38 (4)
H4B0.2582370.8389890.3495130.058*0.38 (4)
H4C0.1187350.7112200.2391910.058*0.38 (4)
H4D0.2089010.8181690.2680520.058*0.62 (4)
H4E0.0779050.6250900.2917920.058*0.62 (4)
H4F0.2174070.7528590.4021130.058*0.62 (4)
C50.7299 (4)0.3460 (4)0.2023 (3)0.0461 (8)
H5A0.8170410.3342930.2624540.097 (9)*
H5B0.7888250.4504880.1603880.097 (9)*
H5C0.6844550.2421500.1398500.097 (9)*
C60.2746 (4)0.3915 (3)0.4059 (2)0.0306 (5)
C70.2650 (4)0.1360 (4)0.5105 (3)0.0387 (7)
H7A0.2268950.1943890.5812270.051 (5)*
H7B0.3523950.0908140.5412660.051 (5)*
H7C0.1597530.0388180.4681510.051 (5)*
C80.4901 (4)0.2398 (4)0.3536 (2)0.0312 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.02068 (7)0.02260 (7)0.01919 (6)0.00823 (5)0.00384 (4)0.00678 (4)
Cl10.0415 (4)0.0448 (4)0.0214 (3)0.0164 (3)0.0078 (2)0.0081 (2)
Cl20.0232 (3)0.0458 (4)0.0396 (3)0.0136 (3)0.0015 (2)0.0125 (3)
Cl30.0420 (4)0.0236 (3)0.0410 (3)0.0114 (3)0.0123 (3)0.0088 (2)
O10.0488 (13)0.0419 (12)0.0622 (14)0.0242 (11)0.0122 (10)0.0258 (10)
O20.0584 (15)0.0519 (14)0.0569 (13)0.0294 (12)0.0344 (11)0.0201 (11)
N10.0342 (13)0.0317 (12)0.0351 (12)0.0088 (10)0.0109 (10)0.0131 (9)
N20.0337 (12)0.0253 (11)0.0357 (11)0.0106 (10)0.0019 (9)0.0054 (9)
N30.0285 (12)0.0289 (11)0.0327 (11)0.0110 (9)0.0066 (9)0.0085 (8)
N40.0331 (12)0.0278 (11)0.0258 (10)0.0103 (9)0.0052 (8)0.0090 (8)
C10.0280 (13)0.0218 (12)0.0303 (12)0.0079 (10)0.0015 (10)0.0040 (9)
C20.0288 (13)0.0236 (12)0.0251 (11)0.0062 (10)0.0009 (9)0.0049 (9)
C30.0453 (18)0.0281 (14)0.0393 (15)0.0110 (13)0.0048 (12)0.0129 (11)
C40.0430 (18)0.0396 (18)0.071 (2)0.0243 (15)0.0078 (16)0.0092 (15)
C50.0368 (17)0.0457 (18)0.062 (2)0.0201 (14)0.0206 (14)0.0134 (15)
C60.0328 (14)0.0288 (13)0.0283 (12)0.0097 (11)0.0043 (10)0.0033 (10)
C70.0433 (17)0.0378 (16)0.0320 (13)0.0087 (13)0.0098 (12)0.0172 (11)
C80.0290 (14)0.0296 (14)0.0329 (13)0.0081 (11)0.0001 (10)0.0082 (10)
Geometric parameters (Å, º) top
Pt1—Cl1i2.3153 (6)N4—C71.464 (3)
Pt1—Cl12.3153 (6)N4—C81.389 (3)
Pt1—Cl2i2.3161 (6)C1—C21.358 (4)
Pt1—Cl22.3161 (6)C1—C61.433 (3)
Pt1—Cl32.3222 (6)C3—H30.89 (3)
Pt1—Cl3i2.3222 (6)C4—H4A0.9600
O1—C81.213 (3)C4—H4B0.9600
O2—C61.213 (3)C4—H4C0.9600
N1—H10.846 (18)C4—H4D0.9600
N1—C21.370 (3)C4—H4E0.9600
N1—C31.335 (4)C4—H4F0.9600
N2—C11.380 (3)C5—H5A0.9600
N2—C31.312 (4)C5—H5B0.9600
N2—C41.469 (4)C5—H5C0.9600
N3—C21.354 (3)C7—H7A0.9600
N3—C51.468 (3)C7—H7B0.9600
N3—C81.389 (3)C7—H7C0.9600
N4—C61.399 (3)
Cl1i—Pt1—Cl1180.0C1—C2—N1107.3 (2)
Cl1—Pt1—Cl289.97 (2)N1—C3—H3125 (2)
Cl1—Pt1—Cl2i90.03 (2)N2—C3—N1109.9 (2)
Cl1i—Pt1—Cl290.03 (2)N2—C3—H3125 (2)
Cl1i—Pt1—Cl2i89.97 (2)N2—C4—H4A109.5
Cl1—Pt1—Cl3i89.93 (2)N2—C4—H4B109.5
Cl1—Pt1—Cl390.07 (2)N2—C4—H4C109.5
Cl1i—Pt1—Cl389.93 (2)H4A—C4—H4B109.5
Cl1i—Pt1—Cl3i90.07 (2)H4A—C4—H4C109.5
Cl2—Pt1—Cl2i180.0H4B—C4—H4C109.5
Cl2i—Pt1—Cl390.52 (3)H4D—C4—H4E109.5
Cl2—Pt1—Cl389.48 (3)H4D—C4—H4F109.5
Cl2i—Pt1—Cl3i89.48 (3)H4E—C4—H4F109.5
Cl2—Pt1—Cl3i90.52 (3)N3—C5—H5A109.5
Cl3i—Pt1—Cl3180.0N3—C5—H5B109.5
C2—N1—H1128 (2)N3—C5—H5C109.5
C3—N1—H1124 (2)H5A—C5—H5B109.5
C3—N1—C2107.7 (2)H5A—C5—H5C109.5
C1—N2—C4125.7 (2)H5B—C5—H5C109.5
C3—N2—C1108.2 (2)O2—C6—N4122.2 (2)
C3—N2—C4126.1 (2)O2—C6—C1126.5 (3)
C2—N3—C5123.2 (2)N4—C6—C1111.2 (2)
C2—N3—C8117.9 (2)N4—C7—H7A109.5
C8—N3—C5118.8 (2)N4—C7—H7B109.5
C6—N4—C7116.2 (2)N4—C7—H7C109.5
C8—N4—C6127.2 (2)H7A—C7—H7B109.5
C8—N4—C7116.5 (2)H7A—C7—H7C109.5
N2—C1—C6131.1 (2)H7B—C7—H7C109.5
C2—C1—N2106.9 (2)O1—C8—N3120.5 (3)
C2—C1—C6122.0 (2)O1—C8—N4122.1 (2)
N3—C2—N1128.6 (2)N4—C8—N3117.3 (2)
N3—C2—C1124.1 (2)
N2—C1—C2—N10.4 (3)C5—N3—C2—N10.8 (4)
N2—C1—C2—N3179.0 (2)C5—N3—C2—C1179.9 (3)
N2—C1—C6—O20.4 (5)C5—N3—C8—O11.5 (4)
N2—C1—C6—N4179.0 (2)C5—N3—C8—N4177.2 (2)
C1—N2—C3—N10.3 (3)C6—N4—C8—O1175.8 (3)
C2—N1—C3—N20.6 (3)C6—N4—C8—N35.4 (4)
C2—N3—C8—O1175.7 (2)C6—C1—C2—N1178.6 (2)
C2—N3—C8—N45.5 (3)C6—C1—C2—N30.7 (4)
C2—C1—C6—O2177.4 (3)C7—N4—C6—O23.3 (4)
C2—C1—C6—N41.2 (3)C7—N4—C6—C1178.1 (2)
C3—N1—C2—N3178.7 (3)C7—N4—C8—O10.3 (4)
C3—N1—C2—C10.6 (3)C7—N4—C8—N3178.4 (2)
C3—N2—C1—C20.0 (3)C8—N3—C2—N1178.0 (3)
C3—N2—C1—C6178.1 (3)C8—N3—C2—C12.8 (4)
C4—N2—C1—C2179.4 (3)C8—N4—C6—O2179.4 (3)
C4—N2—C1—C61.4 (4)C8—N4—C6—C12.0 (4)
C4—N2—C3—N1179.8 (3)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···Cl3ii0.85 (2)2.45 (2)3.296 (2)174 (3)
C3—H3···Cl2ii0.89 (3)2.81 (3)3.455 (3)131 (3)
C5—H5C···Cl20.962.913.563 (3)127
C7—H7B···O1iii0.962.443.346 (4)157
Symmetry codes: (ii) x+1, y+1, z; (iii) x+1, y, z+1.
 

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