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
CCDC reference: 2268577
Key indicators
Structure: I
- Single-crystal X-ray study
- T = 296 K
- Mean (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
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-1
H-purin-9-ium)
hexachloridoplatinum(IV)
top
Crystal data top
(C8H11N4O2)2[PtCl6] | Z = 1 |
Mr = 798.20 | F(000) = 386 |
Triclinic, P1 | Dx = 2.135 Mg m−3 |
a = 7.8800 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.1542 (2) Å | Cell parameters from 4212 reflections |
c = 10.5374 (3) Å | θ = 3.1–29.8° |
α = 95.784 (2)° | µ = 6.34 mm−1 |
β = 91.525 (2)° | T = 296 K |
γ = 112.472 (1)° | Plate, orange |
V = 620.92 (3) Å3 | 0.18 × 0.08 × 0.02 mm |
Data collection top
Bruker Kappa APEXII area-detector diffractometer | 3573 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.035 |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | θmax = 30.0°, θmin = 3.5° |
Tmin = 0.734, Tmax = 1.000 | h = −11→11 |
9764 measured reflections | k = −11→11 |
3616 independent reflections | l = −14→14 |
Refinement top
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.022 | H 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 reflections | Δρmax = 0.45 e Å−3 |
173 parameters | Δρmin = −0.89 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Pt1 | 0.000000 | 0.000000 | 0.000000 | 0.02050 (4) | |
Cl1 | −0.04784 (10) | 0.01026 (9) | 0.21599 (5) | 0.03560 (15) | |
Cl2 | 0.30304 (9) | 0.03978 (10) | 0.04685 (6) | 0.03557 (14) | |
Cl3 | 0.08989 (10) | 0.30803 (8) | 0.01376 (6) | 0.03532 (14) | |
O1 | 0.5394 (3) | 0.1187 (3) | 0.3683 (2) | 0.0474 (5) | |
O2 | 0.1510 (3) | 0.4010 (3) | 0.4685 (2) | 0.0517 (6) | |
N1 | 0.5642 (3) | 0.6187 (3) | 0.1713 (2) | 0.0340 (5) | |
H1 | 0.656 (3) | 0.646 (4) | 0.126 (3) | 0.053 (10)* | |
N2 | 0.3378 (3) | 0.6487 (3) | 0.2696 (2) | 0.0317 (5) | |
N3 | 0.5758 (3) | 0.3628 (3) | 0.2700 (2) | 0.0296 (5) | |
N4 | 0.3502 (3) | 0.2641 (3) | 0.42037 (19) | 0.0289 (5) | |
C1 | 0.3648 (4) | 0.5055 (3) | 0.3126 (2) | 0.0271 (5) | |
C2 | 0.5073 (4) | 0.4880 (3) | 0.2510 (2) | 0.0269 (5) | |
C3 | 0.4589 (4) | 0.7135 (4) | 0.1859 (3) | 0.0378 (7) | |
H3 | 0.475 (4) | 0.812 (4) | 0.150 (3) | 0.046 (9)* | |
C4 | 0.1984 (5) | 0.7171 (4) | 0.3115 (3) | 0.0485 (8) | |
H4A | 0.127241 | 0.645910 | 0.373253 | 0.058* | 0.38 (4) |
H4B | 0.258237 | 0.838989 | 0.349513 | 0.058* | 0.38 (4) |
H4C | 0.118735 | 0.711220 | 0.239191 | 0.058* | 0.38 (4) |
H4D | 0.208901 | 0.818169 | 0.268052 | 0.058* | 0.62 (4) |
H4E | 0.077905 | 0.625090 | 0.291792 | 0.058* | 0.62 (4) |
H4F | 0.217407 | 0.752859 | 0.402113 | 0.058* | 0.62 (4) |
C5 | 0.7299 (4) | 0.3460 (4) | 0.2023 (3) | 0.0461 (8) | |
H5A | 0.817041 | 0.334293 | 0.262454 | 0.097 (9)* | |
H5B | 0.788825 | 0.450488 | 0.160388 | 0.097 (9)* | |
H5C | 0.684455 | 0.242150 | 0.139850 | 0.097 (9)* | |
C6 | 0.2746 (4) | 0.3915 (3) | 0.4059 (2) | 0.0306 (5) | |
C7 | 0.2650 (4) | 0.1360 (4) | 0.5105 (3) | 0.0387 (7) | |
H7A | 0.226895 | 0.194389 | 0.581227 | 0.051 (5)* | |
H7B | 0.352395 | 0.090814 | 0.541266 | 0.051 (5)* | |
H7C | 0.159753 | 0.038818 | 0.468151 | 0.051 (5)* | |
C8 | 0.4901 (4) | 0.2398 (4) | 0.3536 (2) | 0.0312 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pt1 | 0.02068 (7) | 0.02260 (7) | 0.01919 (6) | 0.00823 (5) | 0.00384 (4) | 0.00678 (4) |
Cl1 | 0.0415 (4) | 0.0448 (4) | 0.0214 (3) | 0.0164 (3) | 0.0078 (2) | 0.0081 (2) |
Cl2 | 0.0232 (3) | 0.0458 (4) | 0.0396 (3) | 0.0136 (3) | 0.0015 (2) | 0.0125 (3) |
Cl3 | 0.0420 (4) | 0.0236 (3) | 0.0410 (3) | 0.0114 (3) | 0.0123 (3) | 0.0088 (2) |
O1 | 0.0488 (13) | 0.0419 (12) | 0.0622 (14) | 0.0242 (11) | 0.0122 (10) | 0.0258 (10) |
O2 | 0.0584 (15) | 0.0519 (14) | 0.0569 (13) | 0.0294 (12) | 0.0344 (11) | 0.0201 (11) |
N1 | 0.0342 (13) | 0.0317 (12) | 0.0351 (12) | 0.0088 (10) | 0.0109 (10) | 0.0131 (9) |
N2 | 0.0337 (12) | 0.0253 (11) | 0.0357 (11) | 0.0106 (10) | 0.0019 (9) | 0.0054 (9) |
N3 | 0.0285 (12) | 0.0289 (11) | 0.0327 (11) | 0.0110 (9) | 0.0066 (9) | 0.0085 (8) |
N4 | 0.0331 (12) | 0.0278 (11) | 0.0258 (10) | 0.0103 (9) | 0.0052 (8) | 0.0090 (8) |
C1 | 0.0280 (13) | 0.0218 (12) | 0.0303 (12) | 0.0079 (10) | 0.0015 (10) | 0.0040 (9) |
C2 | 0.0288 (13) | 0.0236 (12) | 0.0251 (11) | 0.0062 (10) | 0.0009 (9) | 0.0049 (9) |
C3 | 0.0453 (18) | 0.0281 (14) | 0.0393 (15) | 0.0110 (13) | 0.0048 (12) | 0.0129 (11) |
C4 | 0.0430 (18) | 0.0396 (18) | 0.071 (2) | 0.0243 (15) | 0.0078 (16) | 0.0092 (15) |
C5 | 0.0368 (17) | 0.0457 (18) | 0.062 (2) | 0.0201 (14) | 0.0206 (14) | 0.0134 (15) |
C6 | 0.0328 (14) | 0.0288 (13) | 0.0283 (12) | 0.0097 (11) | 0.0043 (10) | 0.0033 (10) |
C7 | 0.0433 (17) | 0.0378 (16) | 0.0320 (13) | 0.0087 (13) | 0.0098 (12) | 0.0172 (11) |
C8 | 0.0290 (14) | 0.0296 (14) | 0.0329 (13) | 0.0081 (11) | 0.0001 (10) | 0.0082 (10) |
Geometric parameters (Å, º) top
Pt1—Cl1i | 2.3153 (6) | N4—C7 | 1.464 (3) |
Pt1—Cl1 | 2.3153 (6) | N4—C8 | 1.389 (3) |
Pt1—Cl2i | 2.3161 (6) | C1—C2 | 1.358 (4) |
Pt1—Cl2 | 2.3161 (6) | C1—C6 | 1.433 (3) |
Pt1—Cl3 | 2.3222 (6) | C3—H3 | 0.89 (3) |
Pt1—Cl3i | 2.3222 (6) | C4—H4A | 0.9600 |
O1—C8 | 1.213 (3) | C4—H4B | 0.9600 |
O2—C6 | 1.213 (3) | C4—H4C | 0.9600 |
N1—H1 | 0.846 (18) | C4—H4D | 0.9600 |
N1—C2 | 1.370 (3) | C4—H4E | 0.9600 |
N1—C3 | 1.335 (4) | C4—H4F | 0.9600 |
N2—C1 | 1.380 (3) | C5—H5A | 0.9600 |
N2—C3 | 1.312 (4) | C5—H5B | 0.9600 |
N2—C4 | 1.469 (4) | C5—H5C | 0.9600 |
N3—C2 | 1.354 (3) | C7—H7A | 0.9600 |
N3—C5 | 1.468 (3) | C7—H7B | 0.9600 |
N3—C8 | 1.389 (3) | C7—H7C | 0.9600 |
N4—C6 | 1.399 (3) | | |
| | | |
Cl1i—Pt1—Cl1 | 180.0 | C1—C2—N1 | 107.3 (2) |
Cl1—Pt1—Cl2 | 89.97 (2) | N1—C3—H3 | 125 (2) |
Cl1—Pt1—Cl2i | 90.03 (2) | N2—C3—N1 | 109.9 (2) |
Cl1i—Pt1—Cl2 | 90.03 (2) | N2—C3—H3 | 125 (2) |
Cl1i—Pt1—Cl2i | 89.97 (2) | N2—C4—H4A | 109.5 |
Cl1—Pt1—Cl3i | 89.93 (2) | N2—C4—H4B | 109.5 |
Cl1—Pt1—Cl3 | 90.07 (2) | N2—C4—H4C | 109.5 |
Cl1i—Pt1—Cl3 | 89.93 (2) | H4A—C4—H4B | 109.5 |
Cl1i—Pt1—Cl3i | 90.07 (2) | H4A—C4—H4C | 109.5 |
Cl2—Pt1—Cl2i | 180.0 | H4B—C4—H4C | 109.5 |
Cl2i—Pt1—Cl3 | 90.52 (3) | H4D—C4—H4E | 109.5 |
Cl2—Pt1—Cl3 | 89.48 (3) | H4D—C4—H4F | 109.5 |
Cl2i—Pt1—Cl3i | 89.48 (3) | H4E—C4—H4F | 109.5 |
Cl2—Pt1—Cl3i | 90.52 (3) | N3—C5—H5A | 109.5 |
Cl3i—Pt1—Cl3 | 180.0 | N3—C5—H5B | 109.5 |
C2—N1—H1 | 128 (2) | N3—C5—H5C | 109.5 |
C3—N1—H1 | 124 (2) | H5A—C5—H5B | 109.5 |
C3—N1—C2 | 107.7 (2) | H5A—C5—H5C | 109.5 |
C1—N2—C4 | 125.7 (2) | H5B—C5—H5C | 109.5 |
C3—N2—C1 | 108.2 (2) | O2—C6—N4 | 122.2 (2) |
C3—N2—C4 | 126.1 (2) | O2—C6—C1 | 126.5 (3) |
C2—N3—C5 | 123.2 (2) | N4—C6—C1 | 111.2 (2) |
C2—N3—C8 | 117.9 (2) | N4—C7—H7A | 109.5 |
C8—N3—C5 | 118.8 (2) | N4—C7—H7B | 109.5 |
C6—N4—C7 | 116.2 (2) | N4—C7—H7C | 109.5 |
C8—N4—C6 | 127.2 (2) | H7A—C7—H7B | 109.5 |
C8—N4—C7 | 116.5 (2) | H7A—C7—H7C | 109.5 |
N2—C1—C6 | 131.1 (2) | H7B—C7—H7C | 109.5 |
C2—C1—N2 | 106.9 (2) | O1—C8—N3 | 120.5 (3) |
C2—C1—C6 | 122.0 (2) | O1—C8—N4 | 122.1 (2) |
N3—C2—N1 | 128.6 (2) | N4—C8—N3 | 117.3 (2) |
N3—C2—C1 | 124.1 (2) | | |
| | | |
N2—C1—C2—N1 | −0.4 (3) | C5—N3—C2—N1 | −0.8 (4) |
N2—C1—C2—N3 | 179.0 (2) | C5—N3—C2—C1 | 179.9 (3) |
N2—C1—C6—O2 | −0.4 (5) | C5—N3—C8—O1 | −1.5 (4) |
N2—C1—C6—N4 | −179.0 (2) | C5—N3—C8—N4 | 177.2 (2) |
C1—N2—C3—N1 | 0.3 (3) | C6—N4—C8—O1 | −175.8 (3) |
C2—N1—C3—N2 | −0.6 (3) | C6—N4—C8—N3 | 5.4 (4) |
C2—N3—C8—O1 | 175.7 (2) | C6—C1—C2—N1 | −178.6 (2) |
C2—N3—C8—N4 | −5.5 (3) | C6—C1—C2—N3 | 0.7 (4) |
C2—C1—C6—O2 | 177.4 (3) | C7—N4—C6—O2 | 3.3 (4) |
C2—C1—C6—N4 | −1.2 (3) | C7—N4—C6—C1 | −178.1 (2) |
C3—N1—C2—N3 | −178.7 (3) | C7—N4—C8—O1 | 0.3 (4) |
C3—N1—C2—C1 | 0.6 (3) | C7—N4—C8—N3 | −178.4 (2) |
C3—N2—C1—C2 | 0.0 (3) | C8—N3—C2—N1 | −178.0 (3) |
C3—N2—C1—C6 | 178.1 (3) | C8—N3—C2—C1 | 2.8 (4) |
C4—N2—C1—C2 | −179.4 (3) | C8—N4—C6—O2 | 179.4 (3) |
C4—N2—C1—C6 | −1.4 (4) | C8—N4—C6—C1 | −2.0 (4) |
C4—N2—C3—N1 | 179.8 (3) | | |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···Cl3ii | 0.85 (2) | 2.45 (2) | 3.296 (2) | 174 (3) |
C3—H3···Cl2ii | 0.89 (3) | 2.81 (3) | 3.455 (3) | 131 (3) |
C5—H5C···Cl2 | 0.96 | 2.91 | 3.563 (3) | 127 |
C7—H7B···O1iii | 0.96 | 2.44 | 3.346 (4) | 157 |
Symmetry codes: (ii) −x+1, −y+1, −z; (iii) −x+1, −y, −z+1. |