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The title compound, [Zn(H2O)6][ZnCl3(C8H10N4O2)]2·2H2O, consists of two disordered water mol­ecules, one hexa­hydrated ZnII cation and two [ZnIICl3(caffeine)] anions, which are arranged around an inversion center. The coordination around the hexa­hydrated ZnII cation is octa­hedral. This cation is linked with [ZnIICl3(caffeine)] anions and water mol­ecules via O—H...O hydrogen bonds. Moreover, O—H...O and O—H...Cl hydrogen bonds are co-operative in building up two-dimensional bilayers in which hexa­hydrated ZnII cations are sandwiched between two layers of [ZnIICl3(caffeine)] anions, which are anti-parallel to each other.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805026309/dn6245sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805026309/dn6245Isup2.hkl
Contains datablock I

CCDC reference: 283905

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.003 Å
  • Disorder in solvent or counterion
  • R factor = 0.027
  • wR factor = 0.070
  • Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 11.00 Perc. PLAT417_ALERT_2_C Short Inter D-H..H-D H4WB .. H6B2 .. 2.10 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact Cl1 .. C2 .. 3.24 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O2 .. C5 .. 3.01 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.40 Deg. H6A1 -O6A -H6B1 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 18.20 Deg. H6A1 -O6B -H6B1 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Hexaaquazinc(II) bis[trichloro(3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6- dione-κN9)zincate(II)] dihydrate top
Crystal data top
[Zn(H2O)6][ZnCl3(C8H10N4O2)]2·2H2OF(000) = 952
Mr = 941.40Dx = 1.767 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 890 reflections
a = 8.8699 (6) Åθ = 2.3–34.6°
b = 19.7245 (13) ŵ = 2.53 mm1
c = 10.8701 (7) ÅT = 298 K
β = 111.508 (1)°Prism, colorless
V = 1769.3 (2) Å30.30 × 0.25 × 0.20 mm
Z = 2
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
3178 independent reflections
Radiation source: fine-focus sealed tube2841 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
φ and ω scansθmax = 25.2°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1010
Tmin = 0.473, Tmax = 0.603k = 2321
9304 measured reflectionsl = 139
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0401P)2 + 0.441P]
where P = (Fo2 + 2Fc2)/3
3178 reflections(Δ/σ)max = 0.002
229 parametersΔρmax = 0.29 e Å3
15 restraintsΔρmin = 0.30 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zn10.21334 (3)0.621062 (13)0.21379 (2)0.03608 (10)
Zn20.50000.50000.50000.04515 (12)
Cl10.27639 (9)0.51022 (3)0.22474 (8)0.05735 (19)
Cl20.28042 (7)0.68632 (3)0.35491 (6)0.04439 (15)
Cl30.05272 (7)0.62579 (3)0.24910 (7)0.05225 (17)
O10.89977 (18)0.63678 (9)0.14739 (17)0.0454 (4)
O20.6264 (2)0.69184 (8)0.41716 (16)0.0468 (4)
H5WA0.3296 (13)0.5307 (15)0.253 (2)0.056*
H5WB0.489 (2)0.5177 (13)0.269 (2)0.056*
O30.5211 (3)0.59944 (9)0.5645 (2)0.0594 (5)
H3WA0.557 (4)0.6267 (12)0.522 (3)0.071*
H3WB0.444 (3)0.6180 (13)0.580 (3)0.071*
O40.7462 (2)0.50523 (11)0.5222 (2)0.0655 (6)
H4WA0.771 (4)0.5013 (14)0.455 (2)0.079*
H4WB0.803 (3)0.5343 (13)0.576 (2)0.079*
O50.4274 (2)0.53339 (10)0.30504 (19)0.0541 (5)
N10.7617 (2)0.66264 (10)0.28088 (17)0.0364 (4)
N20.6258 (2)0.64270 (9)0.05206 (17)0.0338 (4)
N30.3292 (2)0.65318 (9)0.02286 (17)0.0347 (4)
N40.3201 (2)0.68648 (9)0.16949 (18)0.0342 (4)
C10.9173 (3)0.66488 (15)0.3938 (2)0.0515 (6)
H1A0.97740.62420.39520.077*
H1B0.89730.66840.47460.077*
H1C0.97860.70350.38520.077*
C20.7699 (2)0.64688 (11)0.1594 (2)0.0349 (5)
C30.6336 (3)0.62276 (15)0.0749 (3)0.0564 (7)
H3A0.59560.57700.09490.085*
H3B0.74370.62560.07020.085*
H3C0.56680.65250.14290.085*
C40.4835 (2)0.65680 (10)0.0695 (2)0.0302 (4)
C50.2358 (3)0.67222 (11)0.0445 (2)0.0360 (5)
H50.12340.67500.00690.043*
C60.2538 (3)0.71007 (15)0.2673 (3)0.0508 (6)
H6A0.14100.72060.22370.076*
H6B0.31120.74990.31050.076*
H6C0.26590.67510.33170.076*
C70.4811 (2)0.67663 (10)0.1878 (2)0.0320 (5)
C80.6223 (3)0.67877 (11)0.3056 (2)0.0351 (5)
O6A0.1101 (3)0.52958 (15)0.1408 (3)0.0694 (8)0.78
H6A10.04510.55870.15030.104*0.78
H6A20.07920.48980.14880.104*0.78
O6B0.1166 (12)0.5262 (6)0.2165 (8)0.0694 (8)0.22
H6B10.06520.54620.14400.104*0.22
H6B20.07740.53580.27470.104*0.22
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.03230 (15)0.04159 (17)0.03358 (16)0.00086 (10)0.01116 (11)0.00244 (10)
Zn20.0455 (2)0.0442 (2)0.0553 (3)0.00373 (17)0.0297 (2)0.00146 (18)
Cl10.0686 (4)0.0388 (3)0.0800 (5)0.0038 (3)0.0455 (4)0.0004 (3)
Cl20.0498 (3)0.0448 (3)0.0420 (3)0.0060 (3)0.0209 (3)0.0048 (2)
Cl30.0314 (3)0.0708 (4)0.0522 (4)0.0016 (3)0.0125 (3)0.0046 (3)
O10.0274 (8)0.0544 (10)0.0534 (11)0.0009 (7)0.0135 (7)0.0028 (8)
O20.0487 (10)0.0583 (11)0.0323 (9)0.0114 (8)0.0136 (7)0.0071 (8)
O30.0744 (14)0.0460 (10)0.0779 (14)0.0022 (9)0.0517 (11)0.0010 (10)
O40.0487 (11)0.0881 (16)0.0705 (14)0.0051 (10)0.0348 (10)0.0148 (11)
O50.0503 (11)0.0621 (12)0.0560 (12)0.0054 (9)0.0266 (9)0.0077 (9)
N10.0282 (9)0.0423 (11)0.0346 (10)0.0050 (8)0.0067 (8)0.0006 (8)
N20.0282 (9)0.0407 (10)0.0331 (10)0.0003 (8)0.0118 (7)0.0013 (8)
N30.0293 (9)0.0428 (10)0.0314 (10)0.0030 (8)0.0106 (7)0.0001 (8)
N40.0321 (9)0.0382 (10)0.0355 (10)0.0029 (7)0.0162 (8)0.0032 (8)
C10.0339 (12)0.0736 (18)0.0390 (14)0.0040 (12)0.0040 (10)0.0000 (12)
C20.0298 (11)0.0345 (12)0.0392 (13)0.0007 (9)0.0111 (9)0.0020 (9)
C30.0377 (13)0.096 (2)0.0381 (14)0.0027 (13)0.0173 (11)0.0106 (13)
C40.0285 (10)0.0307 (10)0.0313 (11)0.0006 (8)0.0108 (8)0.0024 (9)
C50.0294 (11)0.0432 (12)0.0352 (12)0.0013 (9)0.0117 (9)0.0007 (10)
C60.0433 (13)0.0685 (17)0.0493 (15)0.0091 (12)0.0273 (12)0.0194 (13)
C70.0297 (11)0.0333 (11)0.0350 (11)0.0041 (8)0.0143 (9)0.0016 (9)
C80.0369 (12)0.0341 (11)0.0330 (12)0.0089 (9)0.0113 (9)0.0005 (9)
O6A0.0549 (14)0.0688 (15)0.083 (2)0.0092 (12)0.0240 (17)0.0018 (18)
O6B0.0549 (14)0.0688 (15)0.083 (2)0.0092 (12)0.0240 (17)0.0018 (18)
Geometric parameters (Å, º) top
Zn1—N32.0495 (18)N3—C51.345 (3)
Zn1—Cl22.2435 (6)N3—C41.371 (3)
Zn1—Cl32.2497 (7)N4—C51.318 (3)
Zn1—Cl12.2707 (7)N4—C71.381 (3)
Zn2—O3i2.0684 (19)N4—C61.467 (3)
Zn2—O32.0684 (19)C1—H1A0.9600
Zn2—O52.0830 (19)C1—H1B0.9600
Zn2—O5i2.0830 (19)C1—H1C0.9600
Zn2—O42.1101 (19)C3—H3A0.9600
Zn2—O4i2.1101 (19)C3—H3B0.9600
O1—C21.222 (3)C3—H3C0.9600
O2—C81.227 (3)C4—C71.352 (3)
O3—H3WA0.84 (3)C5—H50.9300
O3—H3WB0.85 (3)C6—H6A0.9600
O4—H4WA0.84 (3)C6—H6B0.9600
O4—H4WB0.84 (3)C6—H6C0.9600
O5—H5WA0.84 (3)C7—C81.426 (3)
O5—H5WB0.84 (3)O6A—H6A10.8471
N1—C21.384 (3)O6A—H6A20.8462
N1—C81.395 (3)O6A—H6B10.5264
N1—C11.474 (3)O6B—H6A10.9977
N2—C41.372 (3)O6B—H6A20.9945
N2—C21.382 (3)O6B—H6B10.8489
N2—C31.460 (3)O6B—H6B20.8478
N3—Zn1—Cl2110.79 (5)N1—C1—H1A109.5
N3—Zn1—Cl3105.37 (5)N1—C1—H1B109.5
Cl2—Zn1—Cl3112.59 (3)H1A—C1—H1B109.5
N3—Zn1—Cl1108.00 (6)N1—C1—H1C109.5
Cl2—Zn1—Cl1112.61 (3)H1A—C1—H1C109.5
Cl3—Zn1—Cl1107.10 (3)H1B—C1—H1C109.5
O3i—Zn2—O3180.00 (3)O1—C2—N2121.1 (2)
O3i—Zn2—O589.94 (8)O1—C2—N1121.3 (2)
O3—Zn2—O590.06 (8)N2—C2—N1117.57 (18)
O3i—Zn2—O5i90.06 (8)N2—C3—H3A109.5
O3—Zn2—O5i89.94 (8)N2—C3—H3B109.5
O5—Zn2—O5i180.0H3A—C3—H3B109.5
O3i—Zn2—O492.66 (8)N2—C3—H3C109.5
O3—Zn2—O487.34 (8)H3A—C3—H3C109.5
O5—Zn2—O491.25 (8)H3B—C3—H3C109.5
O5i—Zn2—O488.75 (8)C7—C4—N3110.60 (18)
O3i—Zn2—O4i87.34 (8)C7—C4—N2121.77 (18)
O3—Zn2—O4i92.66 (8)N3—C4—N2127.63 (19)
O5—Zn2—O4i88.75 (8)N4—C5—N3112.98 (19)
O5i—Zn2—O4i91.25 (8)N4—C5—H5123.5
O4—Zn2—O4i180.0N3—C5—H5123.5
Zn2—O3—H3WA115 (2)N4—C6—H6A109.5
Zn2—O3—H3WB120 (2)N4—C6—H6B109.5
H3WA—O3—H3WB109 (2)H6A—C6—H6B109.5
Zn2—O4—H4WA119 (2)N4—C6—H6C109.5
Zn2—O4—H4WB116 (2)H6A—C6—H6C109.5
H4WA—O4—H4WB112 (2)H6B—C6—H6C109.5
Zn2—O5—H5WA121.1 (19)C4—C7—N4106.24 (18)
Zn2—O5—H5WB110.1 (18)C4—C7—C8123.21 (19)
H5WA—O5—H5WB111 (2)N4—C7—C8130.27 (19)
C2—N1—C8126.57 (18)O2—C8—N1122.1 (2)
C2—N1—C1116.12 (19)O2—C8—C7126.2 (2)
C8—N1—C1117.27 (19)N1—C8—C7111.64 (19)
C4—N2—C2118.97 (18)H6A1—O6A—H6A2110.8
C4—N2—C3123.36 (18)H6A1—O6A—H6B15.4
C2—N2—C3117.67 (18)H6A2—O6A—H6B1106.8
C5—N3—C4103.63 (18)H6A1—O6B—H6A288.8
C5—N3—Zn1117.24 (14)H6A1—O6B—H6B118.2
C4—N3—Zn1138.84 (15)H6A2—O6B—H6B174.3
C5—N4—C7106.54 (17)H6A1—O6B—H6B293.9
C5—N4—C6126.0 (2)H6A2—O6B—H6B2126.6
C7—N4—C6127.45 (19)H6B1—O6B—H6B2111.3
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5WA···O6A0.84 (3)1.88 (1)2.725 (4)177 (3)
O5—H5WA···O6B0.84 (3)1.78 (2)2.569 (11)154 (2)
O5—H5WB···Cl1ii0.84 (3)2.36 (1)3.176 (2)162 (2)
O3—H3WA···O20.84 (3)1.96 (3)2.803 (2)176 (3)
O3—H3WB···Cl2iii0.85 (3)2.28 (3)3.1037 (19)167 (3)
O4—H4WA···Cl1ii0.84 (3)2.39 (2)3.180 (2)156 (3)
O4—H4WB···Cl3iv0.84 (3)2.60 (1)3.430 (2)173 (3)
O6A—H6A1···O1v0.852.002.838 (3)170
O6A—H6A2···Cl3vi0.852.573.388 (3)161
O6B—H6B1···O1v0.852.322.821 (9)118
C1—H1B···O20.962.302.736 (3)107
C3—H3B···O10.962.272.703 (3)106
Symmetry codes: (ii) x+1, y+1, z; (iii) x, y, z+1; (iv) x+1, y, z+1; (v) x1, y, z; (vi) x, y+1, z.
 

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