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A new guanine salt hydrate, K+·C5H4N5O·H2O, was obtained and characterized by single-crystal X-ray diffraction in the temperature range 100 K–300 K and compared with that of the previously documented sodium salt hydrate (2Na+·C5H3N5O2−·7H2O) [Gur & Shimon (2015). Acta Cryst. E71, 281–283; Gaydamaka et al. (2019). CrystEngComm, 21, 4484–4492]. Both sodium and potassium salt hydrates have channels. However, the structure of the channels, the cation coordination, the protonation (and, respectively, the charge) of the guanine anions, as well as the role of water molecules in the crystal structure are different for the two salt hydrates. In the crystal structures of the potassium salt, the guanine anions are linked via hydrogen bonds into quartets that form open cylindrical channels in a honeycomb framework. Water molecules `line the walls' of the channels, whereas the potassium cations fill the intra-channel space. This contrasts with the structure of the sodium salt hydrate in which guanine anions form channels with water molecules filling in the channel space together with sodium cations coordinating them. The 1D anionic assembly generated through numerous hydrogen bonds and cation interactions with guanine anions and water molecules is energetically the most distinctive part of the structure of the potassium salt hydrate. In the case of the guanine sodium salt, the structure contains purely inorganic polymeric fragments – sodium cations coordinated to a water molecule forming a 1D polymeric structure and guanine anions interconnecting these polymers via hydrogen bonds with water molecules. The structural differences account for the difference in the anisotropy of strain on temperature variation for the two salt hydrates: whereas in both structures the values of the bulk thermal expansion coefficients are similar in the two structures and the major expansion is observed along the channel axes, the degree of anisotropy for the K salt is more than four times higher than that for the Na salt.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S205252062100754X/xk5085sup1.cif
Contains datablocks 100K, 150K, 200K, 250K, 300K, GuaNa_100K, GuaNa_125K, GuaNa_150K, GuaNa_175K, GuaNa_200K, GuaNa_225K, GuaNa_250K, GuaNa_275K, GuaNa_298K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085100Ksup2.hkl
Contains datablock 100K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085150Ksup3.hkl
Contains datablock 150K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085200Ksup4.hkl
Contains datablock 200K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085250Ksup5.hkl
Contains datablock 250K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085300Ksup6.hkl
Contains datablock 300K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_100Ksup7.hkl
Contains datablock GuaNa_100K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_125Ksup8.hkl
Contains datablock GuaNa_125K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_150Ksup9.hkl
Contains datablock GuaNa_150K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_175Ksup10.hkl
Contains datablock GuaNa_175K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_200Ksup11.hkl
Contains datablock GuaNa_200K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_225Ksup12.hkl
Contains datablock GuaNa_225K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_250Ksup13.hkl
Contains datablock GuaNa_250K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_275Ksup14.hkl
Contains datablock GuaNa_275K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062100754X/xk5085GuaNa_298Ksup15.hkl
Contains datablock GuaNa_298K

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S205252062100754X/xk5085sup16.pdf
Tables S1-S8 and Figs. S1-S3

CCDC references: 2098600; 2098601; 2098602; 2098603; 2098604; 2098605; 2098606; 2098607; 2098608; 2098609; 2098610; 2098611; 2098612; 2098613

Computing details top

Data collection: CrysAlis PRO (Rigaku Oxford Diffraction,2018) for 100K, 150K, 200K, 250K, 300K; STOE X-AREA (Stoe & Cie, 2006) for GuaNa_100K, GuaNa_125K, GuaNa_150K, GuaNa_175K, GuaNa_200K, GuaNa_225K, GuaNa_250K, GuaNa_275K, GuaNa_298K. Cell refinement: CrysAlis PRO (Rigaku Oxford Diffraction,2018) for 100K, 150K, 200K, 250K, 300K; STOE X-AREA (Stoe & Cie, 2006) for GuaNa_100K, GuaNa_125K, GuaNa_150K, GuaNa_175K, GuaNa_200K, GuaNa_225K, GuaNa_250K, GuaNa_275K, GuaNa_298K. Data reduction: CrysAlis PRO (Rigaku Oxford Diffraction,2018) for 100K, 150K, 200K, 250K, 300K; CrysAlis PRO 1.171.38.43d (Rigaku OD, 2015) for GuaNa_100K, GuaNa_125K, GuaNa_150K, GuaNa_175K, GuaNa_200K, GuaNa_225K, GuaNa_250K, GuaNa_275K, GuaNa_298K. Program(s) used to solve structure: SHELXT-2018/3 (Sheldrick, 2018) for 100K, 150K, 200K, 250K, 300K. For all structures, program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2018); molecular graphics: Mercury (Macrae et al., 2020), Vesta(Momma,2011).

potassium{2-amino-6-oxo-1-hydro-purine-7(9)-ide/2-amino-6-oxo-7-hydro-purine-1(3)-ide}monohydrate (100K) top
Crystal data top
C10H12K2N10O4F(000) = 1696
Mr = 414.50Dx = 1.784 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 36.522 (3) ÅCell parameters from 8346 reflections
b = 3.82815 (13) Åθ = 3.5–29.2°
c = 28.639 (2) ŵ = 0.66 mm1
β = 129.573 (12)°T = 100 K
V = 3086.5 (5) Å3Needle, colourless
Z = 80.4 × 0.1 × 0.03 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
4092 independent reflections
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source2972 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
Detector resolution: 10.3457 pixels mm-1θmax = 29.5°, θmin = 3.5°
ω scansh = 4950
Absorption correction: multi-scan
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 55
Tmin = 0.771, Tmax = 1.000l = 3739
25001 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: difference Fourier map
wR(F2) = 0.085Only H-atom coordinates refined
S = 0.91 w = 1/[σ2(Fo2) + (0.0522P)2]
where P = (Fo2 + 2Fc2)/3
4092 reflections(Δ/σ)max < 0.001
271 parametersΔρmax = 0.56 e Å3
3 restraintsΔρmin = 0.41 e Å3
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*/Ueq
K10.49302 (2)0.14591 (10)0.92233 (2)0.01423 (11)
C8A0.33130 (6)0.0483 (5)0.79451 (9)0.0202 (4)
H10.3112 (7)0.117 (6)0.8055 (10)0.024*
C4A0.38670 (6)0.1478 (5)0.79607 (8)0.0132 (4)
C5A0.35054 (6)0.0415 (5)0.73741 (8)0.0132 (4)
C6A0.35565 (6)0.0676 (4)0.69255 (8)0.0121 (4)
C2A0.43023 (5)0.3090 (4)0.77056 (8)0.0114 (4)
N9A0.37440 (5)0.0902 (4)0.83199 (7)0.0181 (3)
N7A0.31513 (5)0.0847 (4)0.73755 (7)0.0158 (3)
H20.2870 (7)0.157 (5)0.7067 (10)0.019*
N1A0.39710 (5)0.2147 (4)0.71205 (6)0.0122 (3)
N3A0.42886 (5)0.2844 (4)0.81566 (6)0.0131 (3)
N2A0.47176 (5)0.4297 (4)0.78451 (8)0.0141 (3)
H30.4918 (7)0.532 (6)0.8205 (10)0.017*
H40.4684 (7)0.540 (6)0.7569 (10)0.017*
O1A0.32538 (4)0.0345 (3)0.63813 (5)0.0140 (3)
O2W0.45280 (4)0.3453 (4)0.94591 (6)0.0156 (3)
H50.4264 (6)0.294 (6)0.9131 (8)0.019*
H60.4454 (7)0.444 (6)0.9646 (9)0.019*
K20.26240 (2)0.52395 (10)0.57122 (2)0.01365 (10)
C8B0.11958 (6)0.7390 (5)0.54214 (9)0.0139 (4)
H70.1217 (7)0.639 (5)0.5737 (9)0.017*
C4B0.09106 (6)0.9982 (4)0.46003 (8)0.0107 (3)
C5B0.13918 (6)0.9361 (4)0.49158 (8)0.0113 (4)
C6B0.16087 (6)1.0483 (4)0.46754 (8)0.0109 (4)
C2B0.08202 (5)1.2711 (4)0.38375 (8)0.0103 (3)
N7B0.15776 (5)0.7691 (4)0.54561 (7)0.0133 (3)
N9B0.07812 (5)0.8705 (4)0.49186 (7)0.0124 (3)
N3B0.06138 (4)1.1680 (4)0.40567 (6)0.0106 (3)
N1B0.12910 (5)1.2117 (4)0.41197 (7)0.0110 (3)
H80.1402 (7)1.297 (5)0.3962 (9)0.013*
N2B0.05656 (5)1.4315 (4)0.32914 (7)0.0133 (3)
H90.0316 (7)1.533 (5)0.3178 (9)0.016*
H100.0723 (7)1.539 (6)0.3204 (9)0.016*
O1B0.20347 (4)1.0190 (3)0.49022 (5)0.0135 (3)
O3W0.22541 (4)0.2952 (4)0.63111 (6)0.0210 (3)
H110.2051 (7)0.486 (3)0.6056 (9)0.025*
H120.2073 (7)0.092 (3)0.6106 (9)0.025*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.01328 (18)0.0148 (2)0.0155 (2)0.00301 (14)0.00959 (17)0.00209 (15)
C8A0.0145 (9)0.0275 (11)0.0176 (10)0.0041 (7)0.0098 (8)0.0014 (8)
C4A0.0113 (8)0.0131 (9)0.0118 (9)0.0012 (6)0.0058 (7)0.0010 (7)
C5A0.0097 (8)0.0140 (9)0.0142 (9)0.0003 (6)0.0068 (7)0.0001 (7)
C6A0.0088 (8)0.0106 (9)0.0122 (9)0.0029 (6)0.0045 (7)0.0018 (7)
C2A0.0103 (8)0.0089 (8)0.0140 (9)0.0026 (6)0.0073 (7)0.0013 (7)
N9A0.0137 (7)0.0262 (9)0.0147 (8)0.0046 (6)0.0092 (7)0.0023 (7)
N7A0.0094 (7)0.0216 (9)0.0128 (8)0.0043 (6)0.0054 (7)0.0022 (6)
N1A0.0100 (6)0.0120 (8)0.0124 (7)0.0008 (5)0.0061 (6)0.0006 (6)
N3A0.0095 (7)0.0148 (8)0.0124 (8)0.0002 (6)0.0058 (6)0.0004 (6)
N2A0.0102 (7)0.0192 (9)0.0107 (8)0.0028 (6)0.0056 (7)0.0008 (6)
O1A0.0098 (6)0.0155 (7)0.0104 (6)0.0004 (5)0.0035 (5)0.0016 (5)
O2W0.0109 (6)0.0206 (7)0.0137 (7)0.0014 (5)0.0072 (5)0.0047 (6)
K20.01048 (18)0.0132 (2)0.0136 (2)0.00032 (14)0.00599 (16)0.00102 (15)
C8B0.0144 (8)0.0133 (9)0.0138 (9)0.0013 (7)0.0089 (8)0.0006 (7)
C4B0.0104 (8)0.0084 (8)0.0122 (9)0.0023 (6)0.0066 (7)0.0030 (7)
C5B0.0101 (8)0.0100 (9)0.0108 (9)0.0003 (6)0.0054 (7)0.0003 (6)
C6B0.0106 (8)0.0071 (8)0.0128 (9)0.0012 (6)0.0063 (7)0.0033 (6)
C2B0.0086 (7)0.0078 (8)0.0121 (9)0.0007 (6)0.0054 (7)0.0031 (6)
N7B0.0121 (7)0.0134 (8)0.0116 (8)0.0009 (6)0.0063 (6)0.0018 (6)
N9B0.0119 (7)0.0124 (7)0.0125 (7)0.0003 (5)0.0076 (6)0.0007 (6)
N3B0.0086 (6)0.0109 (7)0.0109 (7)0.0010 (5)0.0055 (6)0.0015 (6)
N1B0.0084 (6)0.0129 (8)0.0122 (8)0.0014 (5)0.0067 (6)0.0001 (6)
N2B0.0083 (7)0.0164 (8)0.0160 (8)0.0021 (6)0.0082 (7)0.0042 (6)
O1B0.0062 (5)0.0166 (7)0.0142 (6)0.0009 (5)0.0049 (5)0.0010 (5)
O3W0.0123 (6)0.0176 (7)0.0184 (7)0.0023 (5)0.0029 (6)0.0017 (6)
Geometric parameters (Å, º) top
K1—O2W2.7230 (14)O1A—K2v2.6771 (13)
K1—O2Wi2.7698 (14)O2W—H50.835 (16)
K1—N3A2.9012 (16)O2W—H60.828 (17)
K1—N3Bii2.9130 (14)K2—O1B2.6914 (13)
K1—N9Bii3.0276 (16)K2—O1Bv2.7182 (13)
K1—O2Wiii3.0372 (15)K2—O1Bvi2.7336 (14)
K1—N9Biv3.1060 (15)K2—O3W2.9130 (15)
K1—N3Ai3.2339 (15)K2—C6Bv3.4429 (17)
K1—C4Bii3.3042 (18)K2—K2v3.8282 (1)
K1—C4A3.3952 (18)K2—K2i3.8282 (1)
K1—N9A3.4640 (16)K2—K2vi3.9687 (8)
K1—K1v3.8282 (1)K2—K2vii4.1418 (9)
K1—H52.83 (2)K2—H112.83 (2)
C8A—N9A1.326 (2)C8B—N7B1.338 (2)
C8A—N7A1.342 (3)C8B—N9B1.357 (2)
C8A—H11.00 (2)C8B—H70.94 (2)
C4A—N3A1.363 (2)C4B—N9B1.358 (2)
C4A—N9A1.378 (2)C4B—N3B1.368 (2)
C4A—C5A1.380 (3)C4B—C5B1.392 (2)
C5A—N7A1.383 (2)C5B—N7B1.388 (2)
C5A—C6A1.415 (3)C5B—C6B1.407 (3)
C6A—O1A1.268 (2)C6B—O1B1.252 (2)
C6A—N1A1.358 (2)C6B—N1B1.385 (2)
C6A—K2v3.3225 (18)C2B—N3B1.312 (2)
C2A—N3A1.327 (2)C2B—N2B1.354 (2)
C2A—N1A1.349 (2)C2B—N1B1.375 (2)
C2A—N2A1.379 (2)N1B—H80.84 (2)
N7A—H20.87 (2)N2B—H90.84 (2)
N2A—H30.89 (2)N2B—H100.86 (2)
N2A—H40.83 (2)O3W—H110.963 (13)
O1A—K22.6188 (13)O3W—H120.947 (13)
O2W—K1—O2Wi88.36 (4)K1iii—O2W—H662.3 (15)
O2W—K1—N3A70.58 (4)H5—O2W—H6102 (2)
O2Wi—K1—N3A117.26 (4)O1A—K2—O1Ai92.57 (4)
O2W—K1—N3Bii149.72 (4)O1A—K2—O1B169.06 (4)
O2Wi—K1—N3Bii120.73 (4)O1Ai—K2—O1B87.34 (4)
N3A—K1—N3Bii99.67 (4)O1A—K2—O1Bv87.96 (4)
O2W—K1—N9Bii138.51 (4)O1Ai—K2—O1Bv169.16 (4)
O2Wi—K1—N9Bii83.76 (4)O1B—K2—O1Bv90.09 (4)
N3A—K1—N9Bii147.34 (4)O1A—K2—O1Bvi83.09 (4)
N3Bii—K1—N9Bii47.97 (4)O1Ai—K2—O1Bvi88.19 (4)
O2W—K1—O2Wiii83.85 (4)O1B—K2—O1Bvi85.97 (4)
O2Wi—K1—O2Wiii63.08 (4)O1Bv—K2—O1Bvi81.12 (4)
N3A—K1—O2Wiii154.28 (4)O1A—K2—O3W82.81 (4)
N3Bii—K1—O2Wiii101.19 (4)O1Ai—K2—O3W107.90 (4)
N9Bii—K1—O2Wiii56.34 (4)O1B—K2—O3W107.64 (4)
O2W—K1—N9Biv83.05 (4)O1Bv—K2—O3W82.92 (4)
O2Wi—K1—N9Biv139.53 (4)O1Bvi—K2—O3W159.01 (4)
N3A—K1—N9Biv96.94 (4)O1A—K2—C6Ai74.58 (4)
N3Bii—K1—N9Biv69.44 (4)O1Ai—K2—C6Ai21.09 (4)
N9Bii—K1—N9Biv77.22 (3)O1B—K2—C6Ai107.11 (4)
O2Wiii—K1—N9Biv76.68 (4)O1Bv—K2—C6Ai162.54 (4)
O2W—K1—N3Ai121.28 (4)O1Bvi—K2—C6Ai96.75 (4)
O2Wi—K1—N3Ai65.07 (4)O3W—K2—C6Ai94.40 (4)
N3A—K1—N3Ai77.00 (4)O1A—K2—C6Bv102.36 (4)
N3Bii—K1—N3Ai82.02 (4)O1Ai—K2—C6Bv164.94 (4)
N9Bii—K1—N3Ai91.80 (4)O1B—K2—C6Bv78.38 (4)
O2Wiii—K1—N3Ai120.71 (4)O1Bv—K2—C6Bv19.21 (4)
N9Biv—K1—N3Ai149.52 (4)O1Bvi—K2—C6Bv95.47 (4)
O2W—K1—C4Bii147.92 (4)O3W—K2—C6Bv72.55 (4)
O2Wi—K1—C4Bii105.25 (4)C6Ai—K2—C6Bv166.93 (5)
N3A—K1—C4Bii123.94 (5)O1A—K2—K2v44.32 (3)
N3Bii—K1—C4Bii24.39 (4)O1Ai—K2—K2v136.89 (3)
N9Bii—K1—C4Bii24.26 (4)O1B—K2—K2v134.76 (3)
O2Wiii—K1—C4Bii77.16 (4)O1Bv—K2—K2v44.67 (3)
N9Biv—K1—C4Bii67.64 (4)O1Bvi—K2—K2v86.55 (3)
N3Ai—K1—C4Bii90.74 (4)O3W—K2—K2v72.51 (3)
O2W—K1—C4A66.66 (4)C6Ai—K2—K2v118.07 (3)
O2Wi—K1—C4A93.91 (4)C6Bv—K2—K2v58.07 (3)
N3A—K1—C4A23.36 (4)O1A—K2—K2i135.68 (3)
N3Bii—K1—C4A115.13 (4)O1Ai—K2—K2i43.11 (3)
N9Bii—K1—C4A154.34 (4)O1B—K2—K2i45.24 (3)
O2Wiii—K1—C4A143.55 (4)O1Bv—K2—K2i135.33 (3)
N9Biv—K1—C4A118.06 (5)O1Bvi—K2—K2i93.45 (3)
N3Ai—K1—C4A64.43 (4)O3W—K2—K2i107.50 (3)
C4Bii—K1—C4A138.64 (5)C6Ai—K2—K2i61.93 (3)
O2W—K1—N9A52.37 (4)C6Bv—K2—K2i121.93 (3)
O2Wi—K1—N9A76.13 (4)K2v—K2—K2i180.0
N3A—K1—N9A43.82 (4)O1A—K2—K2vi125.66 (3)
N3Bii—K1—N9A137.40 (4)O1Ai—K2—K2vi86.95 (3)
N9Bii—K1—N9A157.25 (4)O1B—K2—K2vi43.40 (3)
O2Wiii—K1—N9A120.56 (4)O1Bv—K2—K2vi83.96 (3)
N9Biv—K1—N9A125.26 (4)O1Bvi—K2—K2vi42.57 (3)
N3Ai—K1—N9A70.22 (4)O3W—K2—K2vi148.06 (3)
C4Bii—K1—N9A158.60 (4)C6Ai—K2—K2vi106.28 (4)
C4A—K1—N9A23.15 (4)C6Bv—K2—K2vi85.93 (3)
O2W—K1—K1v46.32 (3)K2v—K2—K2vi115.853 (12)
O2Wi—K1—K1v134.68 (3)K2i—K2—K2vi64.145 (12)
N3A—K1—K1v55.40 (3)O1A—K2—K2vii84.11 (3)
N3Bii—K1—K1v104.16 (3)O1Ai—K2—K2vii128.59 (3)
N9Bii—K1—K1v127.70 (3)O1B—K2—K2vii87.40 (3)
O2Wiii—K1—K1v104.56 (3)O1Bv—K2—K2vii40.70 (3)
N9Biv—K1—K1v50.47 (3)O1Bvi—K2—K2vii40.42 (3)
N3Ai—K1—K1v132.40 (3)O3W—K2—K2vii122.36 (3)
C4Bii—K1—K1v114.35 (3)C6Ai—K2—K2vii134.72 (3)
C4A—K1—K1v70.66 (3)C6Bv—K2—K2vii56.16 (3)
N9A—K1—K1v74.88 (3)K2v—K2—K2vii59.573 (11)
O2W—K1—H517.2 (3)K2i—K2—K2vii120.424 (11)
O2Wi—K1—H583.3 (4)K2vi—K2—K2vii56.280 (12)
N3A—K1—H559.6 (4)O1A—K2—H11102.0 (3)
N3Bii—K1—H5155.0 (5)O1Ai—K2—H11106.1 (4)
N9Bii—K1—H5152.5 (4)O1B—K2—H1188.5 (3)
O2Wiii—K1—H596.1 (4)O1Bv—K2—H1184.3 (4)
N9Biv—K1—H597.5 (4)O1Bvi—K2—H11164.4 (4)
N3Ai—K1—H5104.5 (4)O3W—K2—H1119.2 (3)
C4Bii—K1—H5164.6 (4)C6Ai—K2—H1198.8 (4)
C4A—K1—H551.1 (4)C6Bv—K2—H1169.1 (4)
N9A—K1—H535.2 (4)K2v—K2—H1187.1 (3)
K1v—K1—H553.5 (4)K2i—K2—H1192.9 (3)
N9A—C8A—N7A113.67 (18)K2vi—K2—H11130.2 (3)
N9A—C8A—H1125.5 (12)K2vii—K2—H11124.8 (4)
N7A—C8A—H1120.8 (12)N7B—C8B—N9B116.90 (17)
N3A—C4A—N9A125.06 (16)N7B—C8B—H7121.4 (12)
N3A—C4A—C5A124.62 (17)N9B—C8B—H7121.7 (12)
N9A—C4A—C5A110.31 (15)N9B—C4B—N3B124.95 (15)
N3A—C4A—K157.53 (9)N9B—C4B—C5B109.77 (15)
N9A—C4A—K181.23 (10)N3B—C4B—C5B125.27 (16)
C5A—C4A—K1139.19 (13)N9B—C4B—K1viii66.38 (9)
C4A—C5A—N7A105.72 (16)N3B—C4B—K1viii61.57 (9)
C4A—C5A—C6A120.46 (15)C5B—C4B—K1viii159.99 (12)
N7A—C5A—C6A133.80 (16)N7B—C5B—C4B108.71 (15)
O1A—C6A—N1A120.25 (17)N7B—C5B—C6B131.18 (15)
O1A—C6A—C5A125.33 (15)C4B—C5B—C6B120.10 (16)
N1A—C6A—C5A114.42 (15)O1B—C6B—N1B119.42 (16)
O1A—C6A—K2v49.43 (8)O1B—C6B—C5B128.28 (16)
N1A—C6A—K2v111.51 (11)N1B—C6B—C5B112.29 (14)
C5A—C6A—K2v110.04 (10)O1B—C6B—K2i45.59 (8)
N3A—C2A—N1A129.04 (16)N1B—C6B—K2i113.94 (11)
N3A—C2A—N2A117.27 (15)C5B—C6B—K2i111.84 (11)
N1A—C2A—N2A113.60 (16)N3B—C2B—N2B120.51 (14)
C8A—N9A—C4A104.08 (15)N3B—C2B—N1B123.62 (16)
C8A—N9A—K1140.82 (13)N2B—C2B—N1B115.80 (16)
C4A—N9A—K175.62 (9)C8B—N7B—C5B102.17 (14)
C8A—N7A—C5A106.22 (15)C8B—N9B—C4B102.45 (14)
C8A—N7A—H2126.0 (14)C8B—N9B—K1viii155.32 (12)
C5A—N7A—H2127.6 (14)C4B—N9B—K1viii89.36 (10)
C2A—N1A—C6A120.32 (16)C8B—N9B—K1ix115.38 (11)
C2A—N3A—C4A111.08 (14)C4B—N9B—K1ix115.65 (10)
C2A—N3A—K1123.98 (11)K1viii—N9B—K1ix77.22 (3)
C4A—N3A—K199.11 (11)C2B—N3B—C4B114.02 (13)
C2A—N3A—K1v114.69 (11)C2B—N3B—K1viii144.94 (11)
C4A—N3A—K1v126.59 (11)C4B—N3B—K1viii94.03 (10)
K1—N3A—K1v77.00 (4)C2B—N1B—C6B124.67 (16)
C2A—N2A—H3115.0 (14)C2B—N1B—H8118.0 (13)
C2A—N2A—H4115.2 (14)C6B—N1B—H8117.1 (13)
H3—N2A—H4113 (2)C2B—N2B—H9115.5 (15)
C6A—O1A—K2142.31 (11)C2B—N2B—H10117.2 (13)
C6A—O1A—K2v109.47 (10)H9—N2B—H10115 (2)
K2—O1A—K2v92.57 (4)C6B—O1B—K2123.87 (11)
K1—O2W—K1v88.36 (4)C6B—O1B—K2i115.20 (11)
K1—O2W—K1iii96.15 (4)K2—O1B—K2i90.09 (4)
K1v—O2W—K1iii116.92 (4)C6B—O1B—K2vi126.65 (11)
K1—O2W—H588.8 (15)K2—O1B—K2vi94.03 (4)
K1v—O2W—H5107.6 (15)K2i—O1B—K2vi98.87 (4)
K1iii—O2W—H5135.3 (15)K2—O3W—H1175.3 (14)
K1—O2W—H6157.7 (16)K2—O3W—H12106.5 (14)
K1v—O2W—H6106.1 (16)H11—O3W—H12104.9 (14)
N3A—C4A—C5A—N7A178.92 (17)N3B—C4B—C5B—N7B177.88 (16)
N9A—C4A—C5A—N7A0.0 (2)K1viii—C4B—C5B—N7B74.1 (4)
K1—C4A—C5A—N7A100.37 (19)N9B—C4B—C5B—C6B179.50 (16)
N3A—C4A—C5A—C6A0.4 (3)N3B—C4B—C5B—C6B0.6 (3)
N9A—C4A—C5A—C6A178.47 (16)K1viii—C4B—C5B—C6B104.4 (4)
K1—C4A—C5A—C6A78.1 (2)N7B—C5B—C6B—O1B0.6 (3)
C4A—C5A—C6A—O1A177.22 (17)C4B—C5B—C6B—O1B178.72 (17)
N7A—C5A—C6A—O1A0.8 (3)N7B—C5B—C6B—N1B178.83 (17)
C4A—C5A—C6A—N1A2.5 (2)C4B—C5B—C6B—N1B0.7 (2)
N7A—C5A—C6A—N1A179.55 (19)N7B—C5B—C6B—K2i49.3 (2)
C4A—C5A—C6A—K2v128.93 (15)C4B—C5B—C6B—K2i128.82 (14)
N7A—C5A—C6A—K2v53.1 (2)N9B—C8B—N7B—C5B0.4 (2)
N7A—C8A—N9A—C4A0.2 (2)C4B—C5B—N7B—C8B0.84 (19)
N7A—C8A—N9A—K184.3 (2)C6B—C5B—N7B—C8B179.10 (19)
N3A—C4A—N9A—C8A179.01 (18)N7B—C8B—N9B—C4B0.2 (2)
C5A—C4A—N9A—C8A0.1 (2)N7B—C8B—N9B—K1viii117.1 (3)
K1—C4A—N9A—C8A139.53 (14)N7B—C8B—N9B—K1ix126.39 (14)
N3A—C4A—N9A—K139.48 (16)N3B—C4B—N9B—C8B178.19 (17)
C5A—C4A—N9A—K1139.42 (15)C5B—C4B—N9B—C8B0.70 (19)
N9A—C8A—N7A—C5A0.2 (2)K1viii—C4B—N9B—C8B158.15 (13)
C4A—C5A—N7A—C8A0.1 (2)N3B—C4B—N9B—K1viii20.05 (17)
C6A—C5A—N7A—C8A178.3 (2)C5B—C4B—N9B—K1viii158.85 (13)
N3A—C2A—N1A—C6A1.0 (3)N3B—C4B—N9B—K1ix55.4 (2)
N2A—C2A—N1A—C6A175.34 (15)C5B—C4B—N9B—K1ix125.67 (12)
O1A—C6A—N1A—C2A177.00 (16)K1viii—C4B—N9B—K1ix75.48 (7)
C5A—C6A—N1A—C2A2.7 (2)N2B—C2B—N3B—C4B177.57 (16)
K2v—C6A—N1A—C2A128.41 (14)N1B—C2B—N3B—C4B0.8 (2)
N1A—C2A—N3A—C4A1.1 (3)N2B—C2B—N3B—K1viii42.2 (3)
N2A—C2A—N3A—C4A177.34 (15)N1B—C2B—N3B—K1viii141.09 (15)
N1A—C2A—N3A—K1116.54 (17)N9B—C4B—N3B—C2B179.32 (16)
N2A—C2A—N3A—K159.7 (2)C5B—C4B—N3B—C2B0.6 (2)
N1A—C2A—N3A—K1v152.81 (15)K1viii—C4B—N3B—C2B158.40 (16)
N2A—C2A—N3A—K1v30.98 (18)N9B—C4B—N3B—K1viii20.92 (18)
N9A—C4A—N3A—C2A179.91 (17)C5B—C4B—N3B—K1viii157.80 (16)
C5A—C4A—N3A—C2A1.3 (3)N3B—C2B—N1B—C6B2.4 (3)
K1—C4A—N3A—C2A131.95 (15)N2B—C2B—N1B—C6B179.26 (16)
N9A—C4A—N3A—K148.14 (19)O1B—C6B—N1B—C2B177.35 (16)
C5A—C4A—N3A—K1130.61 (17)C5B—C6B—N1B—C2B2.2 (2)
N9A—C4A—N3A—K1v32.4 (2)K2i—C6B—N1B—C2B126.30 (14)
C5A—C4A—N3A—K1v148.87 (15)N1B—C6B—O1B—K2155.75 (12)
K1—C4A—N3A—K1v80.52 (10)C5B—C6B—O1B—K224.8 (2)
N1A—C6A—O1A—K2144.22 (14)K2i—C6B—O1B—K2108.53 (13)
C5A—C6A—O1A—K235.5 (3)N1B—C6B—O1B—K2i95.72 (16)
K2v—C6A—O1A—K2122.38 (19)C5B—C6B—O1B—K2i83.7 (2)
N1A—C6A—O1A—K2v93.40 (16)N1B—C6B—O1B—K2vi28.5 (2)
C5A—C6A—O1A—K2v86.91 (18)C5B—C6B—O1B—K2vi152.05 (14)
N9B—C4B—C5B—N7B1.0 (2)K2i—C6B—O1B—K2vi124.24 (15)
Symmetry codes: (i) x, y+1, z; (ii) x+1/2, y+3/2, z+1/2; (iii) x+1, y, z+2; (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1; (vii) x+1/2, y+1/2, z+1; (viii) x1/2, y+3/2, z1/2; (ix) x1/2, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N9A0.84 (2)2.00 (2)2.810 (2)164 (2)
N7A—H2···O3W0.87 (2)1.96 (2)2.820 (2)173 (2)
O3W—H11···N7B0.96 (1)1.83 (2)2.7718 (19)167 (2)
N2A—H3···N3Biv0.89 (2)2.19 (2)3.019 (2)155.5 (19)
N1B—H8···O1Avi0.84 (2)2.13 (2)2.967 (2)173.1 (19)
O3W—H12···N7Bv0.95 (1)1.99 (2)2.907 (2)162 (2)
Symmetry codes: (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1.
potassium{2-amino-6-oxo-1-hydro-purine-7(9)-ide/2-amino-6-oxo-7-hydro-purine-1(3)-ide}monohydrate (150K) top
Crystal data top
C10H12K2N10O4F(000) = 1696
Mr = 414.50Dx = 1.777 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 36.534 (3) ÅCell parameters from 7917 reflections
b = 3.84179 (16) Åθ = 2.8–29.1°
c = 28.656 (2) ŵ = 0.66 mm1
β = 129.598 (12)°T = 150 K
V = 3099.1 (5) Å3Needle, colourless
Z = 80.4 × 0.1 × 0.03 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
4123 independent reflections
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source2877 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
Detector resolution: 10.357 pixels mm-1θmax = 29.6°, θmin = 2.2°
ω scansh = 4950
Absorption correction: multi-scan
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 55
Tmin = 0.743, Tmax = 1.000l = 3739
26051 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: difference Fourier map
wR(F2) = 0.089Only H-atom coordinates refined
S = 0.91 w = 1/[σ2(Fo2) + (0.0522P)2]
where P = (Fo2 + 2Fc2)/3
4123 reflections(Δ/σ)max = 0.003
271 parametersΔρmax = 0.44 e Å3
3 restraintsΔρmin = 0.39 e Å3
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*/Ueq
K10.49295 (2)0.14592 (12)0.92220 (2)0.01886 (11)
C8A0.33139 (7)0.0481 (6)0.79432 (9)0.0262 (5)
H10.3110 (8)0.116 (6)0.8052 (10)0.031*
C4A0.38668 (6)0.1471 (5)0.79592 (8)0.0164 (4)
C5A0.35046 (6)0.0417 (5)0.73728 (8)0.0159 (4)
C6A0.35567 (6)0.0672 (5)0.69258 (8)0.0142 (4)
C2A0.43020 (6)0.3079 (5)0.77046 (8)0.0138 (4)
N9A0.37438 (5)0.0899 (5)0.83175 (7)0.0229 (4)
N7A0.31520 (6)0.0845 (5)0.73740 (7)0.0207 (4)
H20.2881 (8)0.157 (6)0.7073 (10)0.025*
N1A0.39706 (5)0.2135 (4)0.71198 (7)0.0147 (3)
N3A0.42877 (5)0.2836 (4)0.81550 (7)0.0159 (3)
N2A0.47169 (5)0.4278 (4)0.78441 (8)0.0166 (3)
H30.4911 (7)0.532 (6)0.8207 (10)0.020*
H40.4678 (7)0.534 (6)0.7562 (10)0.020*
O1A0.32526 (4)0.0348 (4)0.63802 (6)0.0176 (3)
O2W0.45272 (5)0.3456 (4)0.94584 (6)0.0198 (3)
H50.4272 (6)0.298 (6)0.9135 (8)0.024*
H60.4450 (8)0.438 (6)0.9634 (10)0.024*
K20.26242 (2)0.52427 (11)0.57126 (2)0.01757 (11)
C8B0.11968 (6)0.7399 (5)0.54217 (9)0.0176 (4)
H70.1215 (7)0.640 (6)0.5722 (10)0.021*
C4B0.09110 (6)0.9993 (5)0.46013 (8)0.0133 (4)
C5B0.13923 (6)0.9356 (5)0.49170 (8)0.0136 (4)
C6B0.16094 (6)1.0478 (5)0.46776 (8)0.0139 (4)
C2B0.08208 (6)1.2710 (5)0.38386 (8)0.0127 (4)
N7B0.15777 (5)0.7697 (4)0.54556 (7)0.0166 (3)
N9B0.07821 (5)0.8710 (4)0.49188 (7)0.0152 (3)
N3B0.06140 (5)1.1683 (4)0.40573 (6)0.0128 (3)
N1B0.12920 (5)1.2123 (4)0.41217 (7)0.0131 (3)
H80.1399 (7)1.294 (6)0.3954 (9)0.016*
N2B0.05681 (5)1.4312 (5)0.32953 (7)0.0156 (3)
H90.0320 (8)1.523 (6)0.3173 (10)0.019*
H100.0724 (7)1.540 (6)0.3196 (9)0.019*
O1B0.20352 (4)1.0188 (4)0.49036 (6)0.0172 (3)
O3W0.22530 (5)0.2963 (4)0.63128 (6)0.0281 (4)
H110.2058 (8)0.485 (4)0.6079 (10)0.034*
H120.2097 (8)0.092 (3)0.6118 (10)0.034*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0181 (2)0.0215 (2)0.0189 (2)0.00423 (16)0.01271 (18)0.00296 (17)
C8A0.0193 (10)0.0404 (14)0.0199 (11)0.0075 (9)0.0129 (9)0.0034 (9)
C4A0.0133 (8)0.0206 (10)0.0127 (9)0.0010 (7)0.0071 (7)0.0006 (8)
C5A0.0108 (8)0.0203 (10)0.0143 (9)0.0000 (7)0.0069 (8)0.0000 (7)
C6A0.0106 (8)0.0136 (10)0.0131 (9)0.0028 (6)0.0051 (8)0.0003 (7)
C2A0.0110 (8)0.0136 (10)0.0138 (9)0.0023 (7)0.0065 (7)0.0009 (7)
N9A0.0172 (8)0.0368 (11)0.0158 (8)0.0066 (7)0.0109 (7)0.0031 (7)
N7A0.0126 (8)0.0307 (11)0.0146 (8)0.0065 (7)0.0066 (7)0.0042 (7)
N1A0.0117 (7)0.0191 (9)0.0119 (7)0.0009 (6)0.0068 (6)0.0005 (6)
N3A0.0110 (7)0.0219 (9)0.0116 (8)0.0009 (6)0.0056 (6)0.0006 (6)
N2A0.0120 (7)0.0244 (10)0.0109 (8)0.0039 (6)0.0062 (7)0.0015 (7)
O1A0.0130 (6)0.0211 (8)0.0122 (7)0.0007 (5)0.0050 (5)0.0024 (5)
O2W0.0136 (6)0.0295 (8)0.0148 (7)0.0004 (6)0.0084 (6)0.0053 (6)
K20.01360 (19)0.0189 (2)0.0159 (2)0.00080 (15)0.00738 (17)0.00181 (16)
C8B0.0180 (9)0.0198 (11)0.0157 (10)0.0011 (7)0.0111 (8)0.0015 (8)
C4B0.0120 (8)0.0151 (9)0.0114 (9)0.0019 (7)0.0068 (7)0.0037 (7)
C5B0.0106 (8)0.0155 (10)0.0110 (9)0.0005 (7)0.0052 (7)0.0004 (7)
C6B0.0114 (8)0.0146 (10)0.0128 (9)0.0016 (7)0.0064 (8)0.0037 (7)
C2B0.0105 (8)0.0143 (9)0.0117 (9)0.0015 (7)0.0063 (7)0.0046 (7)
N7B0.0143 (7)0.0194 (9)0.0123 (8)0.0002 (6)0.0067 (6)0.0013 (6)
N9B0.0153 (7)0.0169 (9)0.0149 (8)0.0012 (6)0.0102 (7)0.0008 (6)
N3B0.0100 (7)0.0162 (8)0.0109 (7)0.0013 (6)0.0060 (6)0.0020 (6)
N1B0.0103 (7)0.0178 (9)0.0126 (8)0.0009 (6)0.0079 (6)0.0006 (6)
N2B0.0097 (7)0.0226 (10)0.0152 (8)0.0030 (6)0.0083 (7)0.0055 (6)
O1B0.0081 (6)0.0245 (8)0.0153 (7)0.0024 (5)0.0058 (5)0.0023 (5)
O3W0.0168 (7)0.0245 (9)0.0232 (8)0.0035 (6)0.0035 (6)0.0021 (6)
Geometric parameters (Å, º) top
K1—O2W2.7302 (15)O1A—K2v2.6792 (14)
K1—O2Wi2.7758 (16)O2W—H50.812 (17)
K1—N3A2.9036 (17)O2W—H60.799 (18)
K1—N3Bii2.9140 (15)K2—O1B2.6936 (14)
K1—N9Bii3.0341 (17)K2—O1Bv2.7234 (14)
K1—O2Wiii3.0428 (15)K2—O1Bvi2.7378 (14)
K1—N9Biv3.1152 (16)K2—O3W2.9218 (17)
K1—N3Ai3.2421 (16)K2—C6Bv3.4462 (18)
K1—C4Bii3.3061 (18)K2—K2v3.8418 (1)
K1—C4A3.395 (2)K2—K2i3.8418 (2)
K1—N9A3.4627 (18)K2—K2vi3.9732 (9)
K1—K1v3.8418 (2)K2—K2vii4.1496 (9)
K1—H52.82 (2)K2—H112.86 (2)
C8A—N9A1.323 (3)C8B—N7B1.336 (2)
C8A—N7A1.342 (3)C8B—N9B1.357 (2)
C8A—H11.01 (2)C8B—H70.91 (2)
C4A—N3A1.362 (2)C4B—N9B1.356 (2)
C4A—N9A1.376 (2)C4B—N3B1.368 (2)
C4A—C5A1.380 (3)C4B—C5B1.394 (2)
C5A—N7A1.379 (2)C5B—N7B1.384 (2)
C5A—C6A1.413 (3)C5B—C6B1.407 (3)
C6A—O1A1.272 (2)C6B—O1B1.252 (2)
C6A—N1A1.357 (2)C6B—N1B1.388 (2)
C6A—K2v3.3251 (19)C2B—N3B1.313 (2)
C2A—N3A1.328 (2)C2B—N2B1.350 (2)
C2A—N1A1.349 (2)C2B—N1B1.376 (2)
C2A—N2A1.378 (2)N1B—H80.85 (2)
N7A—H20.84 (2)N2B—H90.82 (2)
N2A—H30.90 (2)N2B—H100.89 (2)
N2A—H40.83 (2)O3W—H110.935 (13)
O1A—K22.6205 (13)O3W—H120.922 (13)
O2W—K1—O2Wi88.49 (4)K1iii—O2W—H662.7 (17)
O2W—K1—N3A70.56 (5)H5—O2W—H6102 (2)
O2Wi—K1—N3A117.33 (4)O1A—K2—O1Ai92.92 (4)
O2W—K1—N3Bii149.65 (5)O1A—K2—O1B169.11 (4)
O2Wi—K1—N3Bii120.65 (5)O1Ai—K2—O1B87.08 (4)
N3A—K1—N3Bii99.73 (5)O1A—K2—O1Bv87.65 (4)
O2W—K1—N9Bii138.51 (4)O1Ai—K2—O1Bv169.22 (4)
O2Wi—K1—N9Bii83.69 (4)O1B—K2—O1Bv90.34 (4)
N3A—K1—N9Bii147.34 (5)O1A—K2—O1Bvi83.15 (4)
N3Bii—K1—N9Bii47.90 (4)O1Ai—K2—O1Bvi88.28 (4)
O2W—K1—O2Wiii83.91 (4)O1B—K2—O1Bvi85.97 (4)
O2Wi—K1—O2Wiii63.05 (5)O1Bv—K2—O1Bvi81.10 (4)
N3A—K1—O2Wiii154.32 (5)O1A—K2—O3W82.79 (4)
N3Bii—K1—O2Wiii101.07 (4)O1Ai—K2—O3W107.88 (4)
N9Bii—K1—O2Wiii56.29 (4)O1B—K2—O3W107.58 (4)
O2W—K1—N9Biv82.91 (4)O1Bv—K2—O3W82.87 (4)
O2Wi—K1—N9Biv139.54 (4)O1Bvi—K2—O3W159.05 (5)
N3A—K1—N9Biv96.84 (5)O1A—K2—C6Ai74.84 (5)
N3Bii—K1—N9Biv69.46 (4)O1Ai—K2—C6Ai21.16 (4)
N9Bii—K1—N9Biv77.32 (4)O1B—K2—C6Ai106.92 (5)
O2Wiii—K1—N9Biv76.72 (4)O1Bv—K2—C6Ai162.48 (4)
O2W—K1—N3Ai121.43 (4)O1Bvi—K2—C6Ai96.83 (4)
O2Wi—K1—N3Ai64.99 (4)O3W—K2—C6Ai94.39 (4)
N3A—K1—N3Ai77.16 (4)O1A—K2—C6Bv102.03 (5)
N3Bii—K1—N3Ai82.02 (4)O1Ai—K2—C6Bv164.91 (4)
N9Bii—K1—N3Ai91.67 (4)O1B—K2—C6Bv78.63 (5)
O2Wiii—K1—N3Ai120.56 (4)O1Bv—K2—C6Bv19.21 (4)
N9Biv—K1—N3Ai149.54 (4)O1Bvi—K2—C6Bv95.44 (4)
O2W—K1—C4Bii147.80 (4)O3W—K2—C6Bv72.48 (4)
O2Wi—K1—C4Bii105.18 (5)C6Ai—K2—C6Bv166.85 (5)
N3A—K1—C4Bii123.99 (5)O1A—K2—K2v44.15 (3)
N3Bii—K1—C4Bii24.38 (4)O1Ai—K2—K2v137.06 (3)
N9Bii—K1—C4Bii24.22 (4)O1B—K2—K2v134.86 (3)
O2Wiii—K1—C4Bii77.04 (4)O1Bv—K2—K2v44.52 (3)
N9Biv—K1—C4Bii67.67 (4)O1Bvi—K2—K2v86.53 (3)
N3Ai—K1—C4Bii90.70 (5)O3W—K2—K2v72.56 (3)
O2W—K1—C4A66.70 (4)C6Ai—K2—K2v118.16 (3)
O2Wi—K1—C4A94.00 (5)C6Bv—K2—K2v57.92 (3)
N3A—K1—C4A23.34 (4)O1A—K2—K2i135.85 (3)
N3Bii—K1—C4A115.15 (4)O1Ai—K2—K2i42.94 (3)
N9Bii—K1—C4A154.31 (5)O1B—K2—K2i45.14 (3)
O2Wiii—K1—C4A143.63 (4)O1Bv—K2—K2i135.48 (3)
N9Biv—K1—C4A117.96 (5)O1Bvi—K2—K2i93.46 (3)
N3Ai—K1—C4A64.57 (5)O3W—K2—K2i107.44 (3)
C4Bii—K1—C4A138.67 (5)C6Ai—K2—K2i61.84 (3)
O2W—K1—N9A52.43 (4)C6Bv—K2—K2i122.08 (3)
O2Wi—K1—N9A76.26 (4)K2v—K2—K2i180.0
N3A—K1—N9A43.76 (4)O1A—K2—K2vi125.70 (4)
N3Bii—K1—N9A137.41 (4)O1Ai—K2—K2vi86.84 (3)
N9Bii—K1—N9A157.28 (5)O1B—K2—K2vi43.42 (3)
O2Wiii—K1—N9A120.67 (4)O1Bv—K2—K2vi84.11 (3)
N9Biv—K1—N9A125.15 (5)O1Bvi—K2—K2vi42.55 (3)
N3Ai—K1—N9A70.32 (4)O3W—K2—K2vi148.02 (3)
C4Bii—K1—N9A158.62 (4)C6Ai—K2—K2vi106.22 (4)
C4A—K1—N9A23.12 (4)C6Bv—K2—K2vi86.08 (4)
O2W—K1—K1v46.24 (3)K2v—K2—K2vi115.882 (13)
O2Wi—K1—K1v134.73 (3)K2i—K2—K2vi64.116 (13)
N3A—K1—K1v55.37 (3)O1A—K2—K2vii83.94 (3)
N3Bii—K1—K1v104.18 (3)O1Ai—K2—K2vii128.68 (3)
N9Bii—K1—K1v127.71 (3)O1B—K2—K2vii87.57 (3)
O2Wiii—K1—K1v104.60 (3)O1Bv—K2—K2vii40.68 (3)
N9Biv—K1—K1v50.40 (3)O1Bvi—K2—K2vii40.42 (3)
N3Ai—K1—K1v132.53 (3)O3W—K2—K2vii122.32 (4)
C4Bii—K1—K1v114.34 (3)C6Ai—K2—K2vii134.78 (4)
C4A—K1—K1v70.63 (4)C6Bv—K2—K2vii56.14 (3)
N9A—K1—K1v74.83 (3)K2v—K2—K2vii59.479 (12)
O2W—K1—H516.7 (4)K2i—K2—K2vii120.519 (12)
O2Wi—K1—H583.9 (5)K2vi—K2—K2vii56.403 (13)
N3A—K1—H559.5 (4)O1A—K2—H11101.3 (3)
N3Bii—K1—H5154.5 (5)O1Ai—K2—H11105.5 (4)
N9Bii—K1—H5152.4 (4)O1B—K2—H1189.1 (3)
O2Wiii—K1—H596.1 (4)O1Bv—K2—H1184.9 (4)
N9Biv—K1—H596.8 (4)O1Bvi—K2—H11165.1 (5)
N3Ai—K1—H5105.2 (4)O3W—K2—H1118.6 (3)
C4Bii—K1—H5164.0 (4)C6Ai—K2—H1198.0 (5)
C4A—K1—H551.3 (4)C6Bv—K2—H1169.8 (5)
N9A—K1—H535.7 (4)K2v—K2—H1187.0 (3)
K1v—K1—H552.8 (5)K2i—K2—H1193.0 (3)
N9A—C8A—N7A113.76 (19)K2vi—K2—H11131.0 (3)
N9A—C8A—H1125.5 (13)K2vii—K2—H11125.4 (4)
N7A—C8A—H1120.7 (13)N7B—C8B—N9B116.83 (18)
N3A—C4A—N9A125.05 (16)N7B—C8B—H7121.7 (13)
N3A—C4A—C5A124.69 (17)N9B—C8B—H7121.4 (13)
N9A—C4A—C5A110.25 (16)N9B—C4B—N3B125.05 (15)
N3A—C4A—K157.64 (9)N9B—C4B—C5B109.54 (16)
N9A—C4A—K181.21 (10)N3B—C4B—C5B125.40 (17)
C5A—C4A—K1139.31 (14)N9B—C4B—K1viii66.59 (9)
C4A—C5A—N7A105.81 (17)N3B—C4B—K1viii61.54 (9)
C4A—C5A—C6A120.32 (16)C5B—C4B—K1viii160.25 (13)
N7A—C5A—C6A133.84 (17)N7B—C5B—C4B108.85 (16)
O1A—C6A—N1A120.23 (17)N7B—C5B—C6B131.14 (15)
O1A—C6A—C5A125.17 (16)C4B—C5B—C6B119.97 (16)
N1A—C6A—C5A114.61 (16)O1B—C6B—N1B119.19 (17)
O1A—C6A—K2v49.48 (9)O1B—C6B—C5B128.40 (17)
N1A—C6A—K2v111.37 (12)N1B—C6B—C5B112.41 (15)
C5A—C6A—K2v109.90 (11)O1B—C6B—K2i45.70 (9)
N3A—C2A—N1A128.95 (16)N1B—C6B—K2i113.54 (12)
N3A—C2A—N2A117.34 (16)C5B—C6B—K2i112.01 (11)
N1A—C2A—N2A113.61 (17)N3B—C2B—N2B120.60 (15)
C8A—N9A—C4A104.04 (16)N3B—C2B—N1B123.64 (16)
C8A—N9A—K1140.73 (15)N2B—C2B—N1B115.70 (17)
C4A—N9A—K175.67 (10)C8B—N7B—C5B102.22 (14)
C8A—N7A—C5A106.14 (16)C8B—N9B—C4B102.54 (15)
C8A—N7A—H2126.6 (15)C8B—N9B—K1viii155.32 (13)
C5A—N7A—H2127.1 (15)C4B—N9B—K1viii89.20 (10)
C2A—N1A—C6A120.24 (16)C8B—N9B—K1ix115.31 (12)
C2A—N3A—C4A111.12 (15)C4B—N9B—K1ix115.77 (11)
C2A—N3A—K1123.91 (11)K1viii—N9B—K1ix77.31 (4)
C4A—N3A—K199.02 (12)C2B—N3B—C4B113.99 (14)
C2A—N3A—K1v114.61 (11)C2B—N3B—K1viii144.92 (12)
C4A—N3A—K1v126.64 (12)C4B—N3B—K1viii94.07 (10)
K1—N3A—K1v77.16 (4)C2B—N1B—C6B124.56 (16)
C2A—N2A—H3113.3 (14)C2B—N1B—H8117.4 (13)
C2A—N2A—H4114.1 (14)C6B—N1B—H8117.9 (13)
H3—N2A—H4115 (2)C2B—N2B—H9116.6 (16)
C6A—O1A—K2142.26 (12)C2B—N2B—H10118.5 (13)
C6A—O1A—K2v109.36 (11)H9—N2B—H10115 (2)
K2—O1A—K2v92.91 (4)C6B—O1B—K2123.76 (12)
K1—O2W—K1v88.49 (4)C6B—O1B—K2i115.09 (12)
K1—O2W—K1iii96.09 (4)K2—O1B—K2i90.34 (4)
K1v—O2W—K1iii116.95 (5)C6B—O1B—K2vi126.68 (12)
K1—O2W—H588.1 (16)K2—O1B—K2vi94.03 (4)
K1v—O2W—H5106.2 (16)K2i—O1B—K2vi98.90 (4)
K1iii—O2W—H5136.7 (16)K2—O3W—H1177.0 (15)
K1—O2W—H6157.6 (18)K2—O3W—H12103.9 (16)
K1v—O2W—H6107.2 (18)H11—O3W—H12109.4 (16)
N3A—C4A—C5A—N7A178.93 (19)N3B—C4B—C5B—N7B178.03 (17)
N9A—C4A—C5A—N7A0.3 (2)K1viii—C4B—C5B—N7B73.6 (4)
K1—C4A—C5A—N7A100.1 (2)N9B—C4B—C5B—C6B179.54 (17)
N3A—C4A—C5A—C6A0.8 (3)N3B—C4B—C5B—C6B0.1 (3)
N9A—C4A—C5A—C6A178.36 (18)K1viii—C4B—C5B—C6B104.6 (4)
K1—C4A—C5A—C6A78.0 (3)N7B—C5B—C6B—O1B0.8 (3)
C4A—C5A—C6A—O1A177.15 (18)C4B—C5B—C6B—O1B178.49 (19)
N7A—C5A—C6A—O1A0.3 (4)N7B—C5B—C6B—N1B178.57 (18)
C4A—C5A—C6A—N1A2.7 (3)C4B—C5B—C6B—N1B0.9 (3)
N7A—C5A—C6A—N1A179.8 (2)N7B—C5B—C6B—K2i49.3 (2)
C4A—C5A—C6A—K2v129.03 (16)C4B—C5B—C6B—K2i128.35 (15)
N7A—C5A—C6A—K2v53.5 (3)N9B—C8B—N7B—C5B0.4 (2)
N7A—C8A—N9A—C4A0.1 (3)C4B—C5B—N7B—C8B1.1 (2)
N7A—C8A—N9A—K184.3 (3)C6B—C5B—N7B—C8B178.9 (2)
N3A—C4A—N9A—C8A179.1 (2)N7B—C8B—N9B—C4B0.4 (2)
C5A—C4A—N9A—C8A0.1 (2)N7B—C8B—N9B—K1viii117.1 (3)
K1—C4A—N9A—C8A139.44 (16)N7B—C8B—N9B—K1ix126.30 (15)
N3A—C4A—N9A—K139.65 (18)N3B—C4B—N9B—C8B178.36 (18)
C5A—C4A—N9A—K1139.53 (16)C5B—C4B—N9B—C8B1.1 (2)
N9A—C8A—N7A—C5A0.3 (3)K1viii—C4B—N9B—C8B158.10 (14)
C4A—C5A—N7A—C8A0.3 (2)N3B—C4B—N9B—K1viii20.26 (19)
C6A—C5A—N7A—C8A178.0 (2)C5B—C4B—N9B—K1viii159.17 (14)
N3A—C2A—N1A—C6A1.0 (3)N3B—C4B—N9B—K1ix55.2 (2)
N2A—C2A—N1A—C6A175.31 (16)C5B—C4B—N9B—K1ix125.35 (13)
O1A—C6A—N1A—C2A177.10 (17)K1viii—C4B—N9B—K1ix75.48 (7)
C5A—C6A—N1A—C2A2.8 (3)N2B—C2B—N3B—C4B177.83 (17)
K2v—C6A—N1A—C2A128.31 (15)N1B—C2B—N3B—C4B0.8 (3)
N1A—C2A—N3A—C4A1.0 (3)N2B—C2B—N3B—K1viii41.9 (3)
N2A—C2A—N3A—C4A177.19 (17)N1B—C2B—N3B—K1viii141.02 (16)
N1A—C2A—N3A—K1116.49 (18)N9B—C4B—N3B—C2B179.58 (18)
N2A—C2A—N3A—K159.7 (2)C5B—C4B—N3B—C2B0.2 (3)
N1A—C2A—N3A—K1v152.74 (16)K1viii—C4B—N3B—C2B158.39 (17)
N2A—C2A—N3A—K1v31.1 (2)N9B—C4B—N3B—K1viii21.19 (19)
N9A—C4A—N3A—C2A179.89 (19)C5B—C4B—N3B—K1viii158.15 (17)
C5A—C4A—N3A—C2A1.0 (3)N3B—C2B—N1B—C6B2.0 (3)
K1—C4A—N3A—C2A131.82 (17)N2B—C2B—N1B—C6B179.18 (17)
N9A—C4A—N3A—K148.3 (2)O1B—C6B—N1B—C2B177.54 (17)
C5A—C4A—N3A—K1130.78 (18)C5B—C6B—N1B—C2B1.9 (3)
N9A—C4A—N3A—K1v32.4 (3)K2i—C6B—N1B—C2B126.54 (15)
C5A—C4A—N3A—K1v148.56 (16)N1B—C6B—O1B—K2155.89 (12)
K1—C4A—N3A—K1v80.66 (11)C5B—C6B—O1B—K224.8 (3)
N1A—C6A—O1A—K2143.91 (15)K2i—C6B—O1B—K2108.72 (14)
C5A—C6A—O1A—K235.9 (3)N1B—C6B—O1B—K2i95.40 (17)
K2v—C6A—O1A—K2122.8 (2)C5B—C6B—O1B—K2i84.0 (2)
N1A—C6A—O1A—K2v93.26 (17)N1B—C6B—O1B—K2vi28.8 (2)
C5A—C6A—O1A—K2v86.88 (19)C5B—C6B—O1B—K2vi151.86 (15)
N9B—C4B—C5B—N7B1.4 (2)K2i—C6B—O1B—K2vi124.17 (16)
Symmetry codes: (i) x, y+1, z; (ii) x+1/2, y+3/2, z+1/2; (iii) x+1, y, z+2; (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1; (vii) x+1/2, y+1/2, z+1; (viii) x1/2, y+3/2, z1/2; (ix) x1/2, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N9A0.81 (2)2.02 (2)2.814 (2)165 (2)
N7A—H2···O3W0.84 (2)1.98 (2)2.822 (2)174 (2)
O3W—H11···N7B0.94 (1)1.86 (2)2.775 (2)165 (2)
N2A—H3···N3Biv0.90 (2)2.20 (2)3.026 (2)153.1 (19)
N1B—H8···O1Avi0.85 (2)2.13 (2)2.972 (2)172.9 (19)
O3W—H12···N7Bv0.92 (1)2.03 (2)2.914 (2)159 (2)
Symmetry codes: (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1.
potassium{2-amino-6-oxo-1-hydro-purine-7(9)-ide/2-amino-6-oxo-7-hydro-purine-1(3)-ide}monohydrate (200K) top
Crystal data top
C10H12K2N10O4F(000) = 1696
Mr = 414.50Dx = 1.769 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 36.553 (3) ÅCell parameters from 8192 reflections
b = 3.85466 (15) Åθ = 2.8–29.2°
c = 28.687 (2) ŵ = 0.66 mm1
β = 129.646 (12)°T = 200 K
V = 3112.3 (5) Å3Needle, colourless
Z = 80.4 × 0.1 × 0.03 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
4145 independent reflections
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source2899 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.055
Detector resolution: 10.3457 pixels mm-1θmax = 29.6°, θmin = 2.2°
ω scansh = 4950
Absorption correction: multi-scan
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 55
Tmin = 0.765, Tmax = 1.000l = 3739
26502 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: difference Fourier map
wR(F2) = 0.074Only H-atom coordinates refined
S = 0.90 w = 1/[σ2(Fo2) + (0.042P)2]
where P = (Fo2 + 2Fc2)/3
4145 reflections(Δ/σ)max = 0.002
271 parametersΔρmax = 0.39 e Å3
3 restraintsΔρmin = 0.27 e Å3
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*/Ueq
K10.49291 (2)0.14581 (10)0.92212 (2)0.02246 (10)
C8A0.33142 (6)0.0477 (6)0.79419 (8)0.0314 (4)
H10.3107 (7)0.121 (5)0.8050 (9)0.038*
C4A0.38660 (5)0.1466 (4)0.79567 (7)0.0185 (3)
C5A0.35045 (5)0.0414 (4)0.73708 (7)0.0186 (3)
C6A0.35558 (5)0.0664 (4)0.69246 (7)0.0159 (3)
C2A0.43016 (5)0.3055 (4)0.77032 (7)0.0154 (3)
N9A0.37434 (5)0.0893 (4)0.83152 (6)0.0273 (4)
N7A0.31521 (5)0.0846 (4)0.73729 (6)0.0247 (3)
H20.2878 (7)0.163 (5)0.7066 (9)0.030*
N1A0.39701 (4)0.2119 (4)0.71192 (6)0.0170 (3)
N3A0.42869 (4)0.2826 (4)0.81532 (6)0.0178 (3)
N2A0.47150 (5)0.4267 (4)0.78418 (7)0.0195 (3)
H30.4910 (6)0.519 (5)0.8198 (8)0.023*
H40.4680 (6)0.537 (5)0.7559 (8)0.023*
O1A0.32516 (4)0.0355 (3)0.63797 (5)0.0197 (3)
O2W0.45264 (4)0.3452 (3)0.94572 (5)0.0239 (3)
H50.4272 (6)0.297 (5)0.9142 (7)0.029*
H60.4448 (7)0.434 (5)0.9632 (8)0.029*
K20.26244 (2)0.52483 (10)0.57127 (2)0.02056 (10)
C8B0.11968 (5)0.7408 (4)0.54194 (7)0.0201 (4)
H70.1222 (6)0.640 (5)0.5732 (8)0.024*
C4B0.09117 (5)1.0001 (4)0.46014 (7)0.0143 (3)
C5B0.13921 (5)0.9360 (4)0.49160 (7)0.0150 (3)
C6B0.16096 (5)1.0481 (4)0.46775 (7)0.0143 (3)
C2B0.08225 (5)1.2707 (4)0.38407 (6)0.0139 (3)
N7B0.15784 (4)0.7697 (4)0.54565 (6)0.0190 (3)
N9B0.07821 (4)0.8718 (4)0.49187 (6)0.0176 (3)
N3B0.06151 (4)1.1690 (3)0.40588 (5)0.0145 (3)
N1B0.12931 (4)1.2115 (4)0.41239 (6)0.0152 (3)
H80.1401 (6)1.290 (5)0.3966 (8)0.018*
N2B0.05693 (5)1.4305 (4)0.32978 (6)0.0187 (3)
H90.0323 (6)1.517 (5)0.3178 (8)0.022*
H100.0736 (6)1.539 (5)0.3206 (8)0.022*
O1B0.20354 (3)1.0183 (3)0.49042 (5)0.0198 (3)
O3W0.22512 (4)0.2973 (4)0.63134 (5)0.0333 (3)
H110.2050 (7)0.484 (3)0.6070 (9)0.040*
H120.2095 (7)0.092 (3)0.6109 (9)0.040*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.02369 (19)0.0238 (2)0.0236 (2)0.00569 (15)0.01686 (17)0.00388 (15)
C8A0.0240 (9)0.0494 (13)0.0238 (10)0.0097 (8)0.0166 (8)0.0034 (8)
C4A0.0154 (7)0.0231 (9)0.0150 (8)0.0004 (6)0.0088 (7)0.0011 (7)
C5A0.0130 (7)0.0233 (9)0.0161 (8)0.0012 (6)0.0077 (7)0.0010 (6)
C6A0.0134 (7)0.0159 (8)0.0142 (8)0.0028 (6)0.0067 (7)0.0003 (6)
C2A0.0136 (7)0.0151 (8)0.0154 (8)0.0017 (6)0.0083 (6)0.0000 (6)
N9A0.0220 (7)0.0442 (10)0.0175 (7)0.0097 (6)0.0134 (6)0.0056 (7)
N7A0.0169 (7)0.0372 (10)0.0177 (7)0.0090 (6)0.0099 (6)0.0045 (6)
N1A0.0146 (6)0.0214 (8)0.0131 (6)0.0002 (5)0.0080 (5)0.0014 (5)
N3A0.0149 (6)0.0232 (8)0.0140 (7)0.0019 (5)0.0085 (6)0.0019 (5)
N2A0.0147 (6)0.0285 (9)0.0134 (7)0.0042 (6)0.0081 (6)0.0019 (6)
O1A0.0160 (5)0.0250 (6)0.0110 (5)0.0016 (4)0.0052 (5)0.0034 (5)
O2W0.0176 (6)0.0362 (8)0.0180 (6)0.0011 (5)0.0114 (5)0.0072 (6)
K20.01789 (17)0.0206 (2)0.01909 (19)0.00095 (14)0.00990 (15)0.00208 (14)
C8B0.0222 (8)0.0222 (9)0.0175 (8)0.0004 (7)0.0133 (7)0.0029 (7)
C4B0.0145 (7)0.0143 (8)0.0140 (8)0.0015 (6)0.0091 (6)0.0032 (6)
C5B0.0139 (7)0.0164 (8)0.0127 (7)0.0005 (6)0.0076 (6)0.0006 (6)
C6B0.0129 (7)0.0135 (8)0.0137 (8)0.0008 (6)0.0071 (6)0.0027 (6)
C2B0.0117 (7)0.0158 (8)0.0124 (7)0.0009 (6)0.0068 (6)0.0035 (6)
N7B0.0182 (6)0.0213 (8)0.0153 (7)0.0011 (5)0.0097 (6)0.0027 (5)
N9B0.0178 (6)0.0205 (7)0.0171 (7)0.0005 (5)0.0124 (6)0.0006 (6)
N3B0.0128 (6)0.0180 (7)0.0128 (6)0.0001 (5)0.0082 (5)0.0005 (5)
N1B0.0132 (6)0.0205 (8)0.0146 (7)0.0007 (5)0.0101 (6)0.0012 (5)
N2B0.0118 (6)0.0266 (9)0.0183 (7)0.0039 (5)0.0099 (6)0.0071 (6)
O1B0.0106 (5)0.0278 (7)0.0181 (6)0.0022 (4)0.0078 (5)0.0028 (5)
O3W0.0196 (6)0.0303 (8)0.0263 (7)0.0041 (5)0.0037 (5)0.0033 (6)
Geometric parameters (Å, º) top
K1—O2W2.7347 (13)O1A—K2v2.6822 (12)
K1—O2Wi2.7834 (14)O2W—H50.802 (15)
K1—N3A2.9063 (14)O2W—H60.796 (16)
K1—N3Bii2.9163 (13)K2—O1B2.6945 (12)
K1—N9Bii3.0366 (14)K2—O1Bv2.7305 (12)
K1—O2Wiii3.0491 (13)K2—O1Bvi2.7411 (12)
K1—N9Biv3.1218 (14)K2—O3W2.9329 (15)
K1—N3Ai3.2518 (14)K2—C6Bv3.4496 (16)
K1—C4Bii3.3095 (16)K2—K2v3.8547 (1)
K1—C4A3.3973 (17)K2—K2i3.8547 (2)
K1—N9A3.4621 (16)K2—K2vi3.9766 (8)
K1—K1v3.8547 (2)K2—K2vii4.1580 (8)
K1—H52.84 (2)K2—H112.87 (2)
C8A—N9A1.320 (2)C8B—N7B1.334 (2)
C8A—N7A1.342 (2)C8B—N9B1.356 (2)
C8A—H11.02 (2)C8B—H70.926 (19)
C4A—N3A1.362 (2)C4B—N9B1.359 (2)
C4A—N9A1.377 (2)C4B—N3B1.367 (2)
C4A—C5A1.379 (2)C4B—C5B1.392 (2)
C5A—N7A1.380 (2)C5B—N7B1.390 (2)
C5A—C6A1.411 (2)C5B—C6B1.407 (2)
C6A—O1A1.2713 (18)C6B—O1B1.2517 (17)
C6A—N1A1.3565 (19)C6B—N1B1.383 (2)
C6A—K2v3.3250 (16)C2B—N3B1.3136 (19)
C2A—N3A1.329 (2)C2B—N2B1.350 (2)
C2A—N1A1.3471 (19)C2B—N1B1.3738 (19)
C2A—N2A1.376 (2)N1B—H80.824 (18)
N7A—H20.864 (19)N2B—H90.802 (19)
N2A—H30.867 (19)N2B—H100.90 (2)
N2A—H40.85 (2)O3W—H110.943 (12)
O1A—K22.6224 (11)O3W—H120.931 (12)
O2W—K1—O2Wi88.62 (4)K1iii—O2W—H662.5 (14)
O2W—K1—N3A70.58 (4)H5—O2W—H6100.8 (19)
O2Wi—K1—N3A117.40 (4)O1A—K2—O1Ai93.21 (3)
O2W—K1—N3Bii149.59 (4)O1A—K2—O1B169.18 (4)
O2Wi—K1—N3Bii120.56 (4)O1Ai—K2—O1B86.90 (4)
N3A—K1—N3Bii99.74 (4)O1A—K2—O1Bv87.36 (4)
O2W—K1—N9Bii138.52 (4)O1Ai—K2—O1Bv169.32 (4)
O2Wi—K1—N9Bii83.58 (4)O1B—K2—O1Bv90.55 (3)
N3A—K1—N9Bii147.31 (4)O1A—K2—O1Bvi83.22 (4)
N3Bii—K1—N9Bii47.88 (4)O1Ai—K2—O1Bvi88.38 (4)
O2W—K1—O2Wiii83.92 (4)O1B—K2—O1Bvi85.97 (4)
O2Wi—K1—O2Wiii63.05 (4)O1Bv—K2—O1Bvi81.09 (4)
N3A—K1—O2Wiii154.34 (4)O1A—K2—O3W82.76 (4)
N3Bii—K1—O2Wiii101.03 (4)O1Ai—K2—O3W107.85 (4)
N9Bii—K1—O2Wiii56.30 (4)O1B—K2—O3W107.52 (4)
O2W—K1—N9Biv82.78 (4)O1Bv—K2—O3W82.81 (4)
O2Wi—K1—N9Biv139.61 (4)O1Bvi—K2—O3W159.07 (4)
N3A—K1—N9Biv96.72 (4)O1A—K2—C6Ai75.09 (4)
N3Bii—K1—N9Biv69.51 (4)O1Ai—K2—C6Ai21.16 (4)
N9Bii—K1—N9Biv77.49 (3)O1B—K2—C6Ai106.76 (4)
O2Wiii—K1—N9Biv76.79 (4)O1Bv—K2—C6Ai162.44 (4)
O2W—K1—N3Ai121.54 (4)O1Bvi—K2—C6Ai96.90 (4)
O2Wi—K1—N3Ai64.89 (4)O3W—K2—C6Ai94.43 (4)
N3A—K1—N3Ai77.28 (3)O1A—K2—C6Bv101.78 (4)
N3Bii—K1—N3Ai82.01 (4)O1Ai—K2—C6Bv164.86 (4)
N9Bii—K1—N3Ai91.51 (4)O1B—K2—C6Bv78.77 (4)
O2Wiii—K1—N3Ai120.45 (4)O1Bv—K2—C6Bv19.22 (3)
N9Biv—K1—N3Ai149.58 (4)O1Bvi—K2—C6Bv95.37 (4)
O2W—K1—C4Bii147.80 (4)O3W—K2—C6Bv72.46 (4)
O2Wi—K1—C4Bii105.09 (4)C6Ai—K2—C6Bv166.86 (4)
N3A—K1—C4Bii123.95 (4)O1A—K2—K2v44.01 (3)
N3Bii—K1—C4Bii24.33 (4)O1Ai—K2—K2v137.22 (2)
N9Bii—K1—C4Bii24.24 (4)O1B—K2—K2v134.90 (3)
O2Wiii—K1—C4Bii77.06 (4)O1Bv—K2—K2v44.35 (2)
N9Biv—K1—C4Bii67.81 (4)O1Bvi—K2—K2v86.53 (3)
N3Ai—K1—C4Bii90.59 (4)O3W—K2—K2v72.59 (3)
O2W—K1—C4A66.73 (4)C6Ai—K2—K2v118.28 (3)
O2Wi—K1—C4A94.09 (4)C6Bv—K2—K2v57.81 (3)
N3A—K1—C4A23.32 (4)O1A—K2—K2i135.99 (3)
N3Bii—K1—C4A115.15 (4)O1Ai—K2—K2i42.79 (2)
N9Bii—K1—C4A154.26 (4)O1B—K2—K2i45.10 (3)
O2Wiii—K1—C4A143.68 (4)O1Bv—K2—K2i135.65 (2)
N9Biv—K1—C4A117.81 (4)O1Bvi—K2—K2i93.48 (3)
N3Ai—K1—C4A64.69 (4)O3W—K2—K2i107.40 (3)
C4Bii—K1—C4A138.61 (4)C6Ai—K2—K2i61.72 (3)
O2W—K1—N9A52.47 (4)C6Bv—K2—K2i122.19 (3)
O2Wi—K1—N9A76.35 (4)K2v—K2—K2i180.0
N3A—K1—N9A43.76 (4)O1A—K2—K2vi125.75 (3)
N3Bii—K1—N9A137.42 (4)O1Ai—K2—K2vi86.78 (3)
N9Bii—K1—N9A157.25 (4)O1B—K2—K2vi43.44 (3)
O2Wiii—K1—N9A120.71 (4)O1Bv—K2—K2vi84.25 (3)
N9Biv—K1—N9A125.02 (4)O1Bvi—K2—K2vi42.53 (2)
N3Ai—K1—N9A70.41 (4)O3W—K2—K2vi147.97 (3)
C4Bii—K1—N9A158.58 (4)C6Ai—K2—K2vi106.15 (3)
C4A—K1—N9A23.13 (4)C6Bv—K2—K2vi86.13 (3)
O2W—K1—K1v46.21 (3)K2v—K2—K2vi115.885 (11)
O2Wi—K1—K1v134.83 (3)K2i—K2—K2vi64.119 (11)
N3A—K1—K1v55.38 (3)O1A—K2—K2vii83.79 (3)
N3Bii—K1—K1v104.17 (3)O1Ai—K2—K2vii128.81 (3)
N9Bii—K1—K1v127.76 (3)O1B—K2—K2vii87.71 (3)
O2Wiii—K1—K1v104.60 (3)O1Bv—K2—K2vii40.64 (2)
N9Biv—K1—K1v50.27 (3)O1Bvi—K2—K2vii40.45 (3)
N3Ai—K1—K1v132.65 (3)O3W—K2—K2vii122.24 (3)
C4Bii—K1—K1v114.35 (3)C6Ai—K2—K2vii134.85 (3)
C4A—K1—K1v70.63 (3)C6Bv—K2—K2vii56.06 (3)
N9A—K1—K1v74.83 (3)K2v—K2—K2vii59.367 (11)
O2W—K1—H516.4 (3)K2i—K2—K2vii120.637 (10)
O2Wi—K1—H583.8 (4)K2vi—K2—K2vii56.518 (11)
N3A—K1—H560.0 (4)O1A—K2—H11101.4 (3)
N3Bii—K1—H5154.9 (4)O1Ai—K2—H11105.8 (4)
N9Bii—K1—H5152.0 (4)O1B—K2—H1188.9 (3)
O2Wiii—K1—H595.7 (4)O1Bv—K2—H1184.5 (4)
N9Biv—K1—H596.6 (4)O1Bvi—K2—H11164.6 (4)
N3Ai—K1—H5105.5 (3)O3W—K2—H1118.7 (2)
C4Bii—K1—H5163.8 (3)C6Ai—K2—H1198.5 (4)
C4A—K1—H551.8 (3)C6Bv—K2—H1169.4 (4)
N9A—K1—H536.0 (3)K2v—K2—H1186.8 (3)
K1v—K1—H553.0 (4)K2i—K2—H1193.2 (3)
N9A—C8A—N7A113.76 (16)K2vi—K2—H11130.7 (3)
N9A—C8A—H1126.1 (11)K2vii—K2—H11124.9 (4)
N7A—C8A—H1120.1 (11)N7B—C8B—N9B117.31 (15)
N3A—C4A—N9A124.97 (14)N7B—C8B—H7120.3 (11)
N3A—C4A—C5A124.66 (15)N9B—C8B—H7122.4 (11)
N9A—C4A—C5A110.37 (14)N9B—C4B—N3B125.00 (13)
N3A—C4A—K157.66 (8)N9B—C4B—C5B109.62 (13)
N9A—C4A—K181.08 (9)N3B—C4B—C5B125.37 (14)
C5A—C4A—K1139.25 (12)N9B—C4B—K1viii66.55 (8)
N7A—C5A—C4A105.62 (14)N3B—C4B—K1viii61.50 (7)
N7A—C5A—C6A133.87 (14)C5B—C4B—K1viii160.38 (11)
C4A—C5A—C6A120.48 (14)N7B—C5B—C4B108.84 (14)
O1A—C6A—N1A120.32 (15)N7B—C5B—C6B131.08 (13)
O1A—C6A—C5A125.18 (14)C4B—C5B—C6B120.04 (14)
N1A—C6A—C5A114.50 (13)O1B—C6B—N1B119.36 (14)
O1A—C6A—K2v49.61 (7)O1B—C6B—C5B128.32 (14)
N1A—C6A—K2v111.35 (10)N1B—C6B—C5B112.32 (13)
C5A—C6A—K2v109.93 (10)O1B—C6B—K2i45.89 (8)
N3A—C2A—N1A128.94 (14)N1B—C6B—K2i113.46 (10)
N3A—C2A—N2A117.35 (14)C5B—C6B—K2i112.07 (10)
N1A—C2A—N2A113.64 (14)N3B—C2B—N2B120.42 (13)
C8A—N9A—C4A104.05 (14)N3B—C2B—N1B123.65 (14)
C8A—N9A—K1140.77 (14)N2B—C2B—N1B115.87 (14)
C4A—N9A—K175.79 (9)C8B—N7B—C5B101.90 (12)
C8A—N7A—C5A106.21 (14)C8B—N9B—C4B102.31 (13)
C8A—N7A—H2126.9 (13)C8B—N9B—K1viii155.54 (11)
C5A—N7A—H2126.8 (13)C4B—N9B—K1viii89.20 (9)
C2A—N1A—C6A120.31 (14)C8B—N9B—K1ix115.17 (11)
C2A—N3A—C4A111.04 (13)C4B—N9B—K1ix115.82 (9)
C2A—N3A—K1123.78 (10)K1viii—N9B—K1ix77.49 (3)
C4A—N3A—K199.02 (10)C2B—N3B—C4B113.89 (12)
C2A—N3A—K1v114.71 (10)C2B—N3B—K1viii145.03 (10)
C4A—N3A—K1v126.63 (10)C4B—N3B—K1viii94.17 (9)
K1—N3A—K1v77.28 (3)C2B—N1B—C6B124.70 (14)
C2A—N2A—H3114.0 (12)C2B—N1B—H8118.1 (12)
C2A—N2A—H4115.1 (12)C6B—N1B—H8117.1 (12)
H3—N2A—H4115.3 (18)C2B—N2B—H9116.0 (14)
C6A—O1A—K2142.29 (10)C2B—N2B—H10116.9 (11)
C6A—O1A—K2v109.22 (9)H9—N2B—H10117.6 (18)
K2—O1A—K2v93.21 (3)C6B—O1B—K2123.91 (10)
K1—O2W—K1v88.62 (4)C6B—O1B—K2i114.89 (10)
K1—O2W—K1iii96.09 (4)K2—O1B—K2i90.55 (3)
K1v—O2W—K1iii116.95 (4)C6B—O1B—K2vi126.59 (10)
K1—O2W—H588.9 (14)K2—O1B—K2vi94.03 (3)
K1v—O2W—H5107.5 (14)K2i—O1B—K2vi98.92 (4)
K1iii—O2W—H5135.4 (14)K2—O3W—H1176.7 (13)
K1—O2W—H6157.0 (15)K2—O3W—H12102.3 (13)
K1v—O2W—H6107.8 (15)H11—O3W—H12107.7 (13)
N3A—C4A—C5A—N7A178.87 (16)N3B—C4B—C5B—N7B177.98 (15)
N9A—C4A—C5A—N7A0.2 (2)K1viii—C4B—C5B—N7B73.6 (4)
K1—C4A—C5A—N7A100.05 (17)N9B—C4B—C5B—C6B179.49 (14)
N3A—C4A—C5A—C6A0.8 (3)N3B—C4B—C5B—C6B0.0 (2)
N9A—C4A—C5A—C6A178.27 (15)K1viii—C4B—C5B—C6B104.4 (3)
K1—C4A—C5A—C6A78.1 (2)N7B—C5B—C6B—O1B1.0 (3)
N7A—C5A—C6A—O1A0.3 (3)C4B—C5B—C6B—O1B178.49 (16)
C4A—C5A—C6A—O1A177.18 (16)N7B—C5B—C6B—N1B178.58 (16)
N7A—C5A—C6A—N1A179.95 (18)C4B—C5B—C6B—N1B1.1 (2)
C4A—C5A—C6A—N1A2.6 (2)N7B—C5B—C6B—K2i49.5 (2)
N7A—C5A—C6A—K2v53.7 (2)C4B—C5B—C6B—K2i128.04 (13)
C4A—C5A—C6A—K2v128.81 (14)N9B—C8B—N7B—C5B0.55 (19)
N7A—C8A—N9A—C4A0.3 (2)C4B—C5B—N7B—C8B1.18 (17)
N7A—C8A—N9A—K184.3 (2)C6B—C5B—N7B—C8B178.90 (17)
N3A—C4A—N9A—C8A179.09 (18)N7B—C8B—N9B—C4B0.31 (19)
C5A—C4A—N9A—C8A0.1 (2)N7B—C8B—N9B—K1viii116.7 (2)
K1—C4A—N9A—C8A139.50 (14)N7B—C8B—N9B—K1ix126.21 (13)
N3A—C4A—N9A—K139.60 (16)N3B—C4B—N9B—C8B178.40 (15)
C5A—C4A—N9A—K1139.44 (14)C5B—C4B—N9B—C8B1.06 (17)
N9A—C8A—N7A—C5A0.4 (2)K1viii—C4B—N9B—C8B158.23 (12)
C4A—C5A—N7A—C8A0.3 (2)N3B—C4B—N9B—K1viii20.17 (15)
C6A—C5A—N7A—C8A178.1 (2)C5B—C4B—N9B—K1viii159.29 (11)
N3A—C2A—N1A—C6A1.2 (3)N3B—C4B—N9B—K1ix55.50 (18)
N2A—C2A—N1A—C6A175.71 (14)C5B—C4B—N9B—K1ix125.04 (11)
O1A—C6A—N1A—C2A176.99 (14)K1viii—C4B—N9B—K1ix75.67 (6)
C5A—C6A—N1A—C2A2.8 (2)N2B—C2B—N3B—C4B177.75 (14)
K2v—C6A—N1A—C2A128.27 (13)N1B—C2B—N3B—C4B0.6 (2)
N1A—C2A—N3A—C4A0.7 (2)N2B—C2B—N3B—K1viii41.7 (2)
N2A—C2A—N3A—C4A177.57 (14)N1B—C2B—N3B—K1viii141.18 (13)
N1A—C2A—N3A—K1116.64 (16)N9B—C4B—N3B—C2B179.68 (15)
N2A—C2A—N3A—K160.22 (18)C5B—C4B—N3B—C2B0.3 (2)
N1A—C2A—N3A—K1v152.44 (14)K1viii—C4B—N3B—C2B158.58 (14)
N2A—C2A—N3A—K1v30.70 (17)N9B—C4B—N3B—K1viii21.10 (16)
N9A—C4A—N3A—C2A179.80 (16)C5B—C4B—N3B—K1viii158.28 (14)
C5A—C4A—N3A—C2A0.9 (2)N3B—C2B—N1B—C6B2.0 (2)
K1—C4A—N3A—C2A131.62 (14)N2B—C2B—N1B—C6B179.21 (14)
N9A—C4A—N3A—K148.18 (18)O1B—C6B—N1B—C2B177.55 (14)
C5A—C4A—N3A—K1130.72 (16)C5B—C6B—N1B—C2B2.0 (2)
N9A—C4A—N3A—K1v32.6 (2)K2i—C6B—N1B—C2B126.34 (13)
C5A—C4A—N3A—K1v148.47 (14)N1B—C6B—O1B—K2155.84 (10)
K1—C4A—N3A—K1v80.81 (9)C5B—C6B—O1B—K224.6 (2)
N1A—C6A—O1A—K2143.56 (13)K2i—C6B—O1B—K2108.95 (11)
C5A—C6A—O1A—K236.2 (3)N1B—C6B—O1B—K2i95.21 (14)
K2v—C6A—O1A—K2123.22 (17)C5B—C6B—O1B—K2i84.32 (18)
N1A—C6A—O1A—K2v93.22 (14)N1B—C6B—O1B—K2vi28.6 (2)
C5A—C6A—O1A—K2v87.02 (17)C5B—C6B—O1B—K2vi151.82 (13)
N9B—C4B—C5B—N7B1.47 (18)K2i—C6B—O1B—K2vi123.86 (13)
Symmetry codes: (i) x, y+1, z; (ii) x+1/2, y+3/2, z+1/2; (iii) x+1, y, z+2; (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1; (vii) x+1/2, y+1/2, z+1; (viii) x1/2, y+3/2, z1/2; (ix) x1/2, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N9A0.80 (2)2.04 (2)2.8162 (19)164 (2)
N7A—H2···O3W0.864 (19)1.965 (19)2.8254 (18)173.3 (19)
O3W—H11···N7B0.94 (1)1.85 (1)2.7734 (18)167 (2)
N2A—H3···N3Biv0.867 (19)2.224 (19)3.0376 (19)156.1 (17)
N1B—H8···O1Avi0.824 (18)2.158 (19)2.9793 (18)174.1 (16)
O3W—H12···N7Bv0.93 (1)2.03 (2)2.9175 (19)160 (2)
Symmetry codes: (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1.
potassium{2-amino-6-oxo-1-hydro-purine-7(9)-ide/2-amino-6-oxo-7-hydro-purine-1(3)-ide}monohydrate (250K) top
Crystal data top
C10H12K2N10O4F(000) = 1696
Mr = 414.50Dx = 1.760 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 36.575 (3) ÅCell parameters from 7629 reflections
b = 3.86969 (17) Åθ = 2.8–29.0°
c = 28.723 (2) ŵ = 0.65 mm1
β = 129.689 (13)°T = 250 K
V = 3128.3 (6) Å3Needle, colourless
Z = 80.4 × 0.1 × 0.03 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
4166 independent reflections
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source2793 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.057
Detector resolution: 10.3457 pixels mm-1θmax = 29.5°, θmin = 2.2°
ω scansh = 4950
Absorption correction: multi-scan
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 55
Tmin = 0.824, Tmax = 1.000l = 3739
26650 measured reflections
Refinement top
Refinement on F2Secondary atom site location: structure-invariant direct methods
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Only H-atom coordinates refined
wR(F2) = 0.074 w = 1/[σ2(Fo2) + (0.040P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.90(Δ/σ)max = 0.002
4166 reflectionsΔρmax = 0.36 e Å3
271 parametersΔρmin = 0.26 e Å3
3 restraints
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*/Ueq
K10.49288 (2)0.14562 (11)0.92197 (2)0.02776 (11)
C8A0.33157 (6)0.0488 (6)0.79405 (9)0.0382 (5)
H10.3110 (7)0.112 (5)0.8048 (9)0.046*
C4A0.38658 (5)0.1457 (5)0.79545 (7)0.0215 (4)
C5A0.35047 (5)0.0397 (5)0.73699 (7)0.0222 (4)
C6A0.35565 (5)0.0651 (4)0.69240 (7)0.0191 (4)
C2A0.43006 (5)0.3043 (4)0.77019 (7)0.0181 (3)
N9A0.37444 (5)0.0883 (4)0.83135 (6)0.0330 (4)
N7A0.31527 (5)0.0850 (4)0.73722 (7)0.0298 (4)
H20.2875 (7)0.165 (5)0.7066 (9)0.036*
N1A0.39695 (4)0.2106 (4)0.71179 (6)0.0201 (3)
N3A0.42860 (4)0.2811 (4)0.81505 (6)0.0211 (3)
N2A0.47146 (5)0.4254 (4)0.78408 (7)0.0239 (3)
H30.4904 (6)0.525 (5)0.8189 (9)0.029*
H40.4673 (6)0.535 (5)0.7554 (9)0.029*
O1A0.32511 (4)0.0363 (3)0.63800 (5)0.0239 (3)
O2W0.45249 (4)0.3453 (4)0.94558 (5)0.0293 (3)
H50.4273 (6)0.292 (5)0.9134 (8)0.035*
H60.4461 (7)0.440 (5)0.9641 (8)0.035*
K20.26246 (2)0.52549 (10)0.57127 (2)0.02487 (10)
C8B0.11971 (6)0.7421 (5)0.54180 (8)0.0241 (4)
H70.1220 (6)0.642 (5)0.5733 (8)0.029*
C4B0.09129 (5)0.9999 (4)0.46022 (7)0.0167 (3)
C5B0.13925 (5)0.9364 (4)0.49163 (7)0.0177 (3)
C6B0.16105 (5)1.0478 (4)0.46789 (7)0.0175 (3)
C2B0.08229 (5)1.2700 (4)0.38422 (7)0.0163 (3)
N7B0.15785 (4)0.7706 (4)0.54546 (6)0.0229 (3)
N9B0.07833 (4)0.8728 (4)0.49191 (6)0.0211 (3)
N3B0.06157 (4)1.1685 (4)0.40594 (5)0.0173 (3)
N1B0.12934 (4)1.2117 (4)0.41264 (6)0.0182 (3)
H80.1395 (6)1.290 (5)0.3955 (8)0.022*
N2B0.05707 (5)1.4302 (4)0.33011 (6)0.0223 (3)
H90.0322 (7)1.521 (5)0.3177 (8)0.027*
H100.0735 (6)1.539 (5)0.3212 (8)0.027*
O1B0.20352 (3)1.0181 (3)0.49047 (5)0.0237 (3)
O3W0.22499 (4)0.2984 (4)0.63148 (6)0.0410 (4)
H110.2039 (7)0.482 (3)0.6079 (9)0.049*
H120.2090 (7)0.093 (3)0.6120 (9)0.049*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0295 (2)0.0294 (2)0.0295 (2)0.00704 (16)0.02116 (18)0.00482 (17)
C8A0.0301 (10)0.0605 (15)0.0289 (10)0.0124 (9)0.0212 (9)0.0042 (9)
C4A0.0184 (8)0.0276 (9)0.0162 (8)0.0000 (7)0.0099 (7)0.0000 (7)
C5A0.0156 (8)0.0289 (10)0.0181 (8)0.0018 (7)0.0089 (7)0.0012 (7)
C6A0.0161 (8)0.0193 (9)0.0168 (8)0.0031 (6)0.0082 (7)0.0005 (6)
C2A0.0158 (7)0.0184 (9)0.0173 (8)0.0016 (6)0.0093 (7)0.0001 (7)
N9A0.0264 (8)0.0530 (11)0.0218 (8)0.0121 (7)0.0164 (7)0.0068 (7)
N7A0.0199 (7)0.0452 (10)0.0223 (8)0.0106 (7)0.0126 (7)0.0054 (7)
N1A0.0165 (6)0.0261 (8)0.0152 (7)0.0001 (5)0.0089 (6)0.0020 (6)
N3A0.0168 (6)0.0292 (8)0.0145 (7)0.0024 (6)0.0086 (6)0.0023 (6)
N2A0.0185 (7)0.0344 (9)0.0168 (7)0.0062 (6)0.0104 (6)0.0040 (6)
O1A0.0193 (6)0.0301 (7)0.0138 (6)0.0022 (5)0.0066 (5)0.0054 (5)
O2W0.0223 (6)0.0433 (8)0.0222 (7)0.0010 (6)0.0142 (5)0.0094 (6)
K20.02199 (18)0.0246 (2)0.0230 (2)0.00140 (15)0.01204 (16)0.00258 (15)
C8B0.0260 (9)0.0277 (10)0.0205 (9)0.0003 (7)0.0158 (8)0.0029 (7)
C4B0.0172 (7)0.0175 (8)0.0160 (8)0.0020 (6)0.0110 (7)0.0036 (6)
C5B0.0162 (7)0.0198 (9)0.0151 (8)0.0001 (6)0.0091 (7)0.0001 (6)
C6B0.0151 (8)0.0174 (8)0.0176 (8)0.0007 (6)0.0093 (7)0.0033 (6)
C2B0.0141 (7)0.0176 (8)0.0148 (8)0.0009 (6)0.0081 (7)0.0037 (6)
N7B0.0217 (7)0.0258 (8)0.0190 (7)0.0015 (6)0.0119 (6)0.0037 (6)
N9B0.0214 (7)0.0255 (8)0.0200 (7)0.0008 (6)0.0148 (6)0.0013 (6)
N3B0.0143 (6)0.0221 (7)0.0152 (7)0.0004 (5)0.0093 (6)0.0009 (6)
N1B0.0144 (6)0.0245 (8)0.0164 (7)0.0003 (5)0.0102 (6)0.0023 (6)
N2B0.0140 (7)0.0320 (9)0.0213 (7)0.0044 (6)0.0115 (6)0.0084 (6)
O1B0.0122 (5)0.0333 (7)0.0217 (6)0.0018 (5)0.0090 (5)0.0030 (5)
O3W0.0239 (7)0.0380 (9)0.0337 (8)0.0050 (6)0.0057 (6)0.0043 (6)
Geometric parameters (Å, º) top
K1—O2W2.7441 (14)O1A—K2v2.6873 (12)
K1—O2Wi2.7933 (14)O2W—H50.811 (15)
K1—N3A2.9093 (15)O2W—H60.795 (16)
K1—N3Bii2.9186 (13)K2—O1B2.6978 (12)
K1—N9Bii3.0424 (15)K2—O1Bv2.7382 (13)
K1—O2Wiii3.0583 (14)K2—O1Bvi2.7459 (13)
K1—N9Biv3.1320 (14)K2—O3W2.9443 (16)
K1—N3Ai3.2646 (14)K2—C6Bv3.4530 (16)
K1—C4Bii3.3157 (16)K2—K2i3.8697 (2)
K1—C4A3.3982 (18)K2—K2v3.8697 (2)
K1—N9A3.4582 (17)K2—K2vi3.9809 (8)
K1—K1i3.8697 (2)K2—K2vii4.1682 (8)
K1—H52.82 (2)K2—H112.93 (2)
C8A—N9A1.320 (2)C8B—N7B1.335 (2)
C8A—N7A1.340 (2)C8B—N9B1.353 (2)
C8A—H11.01 (2)C8B—H70.937 (19)
C4A—N3A1.359 (2)C4B—N9B1.359 (2)
C4A—N9A1.376 (2)C4B—N3B1.369 (2)
C4A—C5A1.378 (2)C4B—C5B1.389 (2)
C5A—N7A1.379 (2)C5B—N7B1.386 (2)
C5A—C6A1.413 (2)C5B—C6B1.408 (2)
C6A—O1A1.2704 (19)C6B—O1B1.2489 (18)
C6A—N1A1.354 (2)C6B—N1B1.384 (2)
C6A—K2v3.3296 (17)C2B—N3B1.3121 (19)
C2A—N3A1.326 (2)C2B—N2B1.349 (2)
C2A—N1A1.348 (2)C2B—N1B1.3728 (19)
C2A—N2A1.378 (2)N1B—H80.840 (18)
N7A—H20.871 (19)N2B—H90.815 (19)
N2A—H30.862 (19)N2B—H100.89 (2)
N2A—H40.85 (2)O3W—H110.945 (12)
O1A—K22.6264 (12)O3W—H120.933 (13)
O2W—K1—O2Wi88.66 (4)K1iii—O2W—H661.4 (15)
O2W—K1—N3A70.62 (4)H5—O2W—H6106 (2)
O2Wi—K1—N3A117.41 (4)O1A—K2—O1Ai93.47 (4)
O2W—K1—N3Bii149.66 (4)O1A—K2—O1B169.29 (4)
O2Wi—K1—N3Bii120.43 (4)O1Ai—K2—O1B86.72 (4)
N3A—K1—N3Bii99.79 (4)O1A—K2—O1Bv87.10 (4)
O2W—K1—N9Bii138.50 (4)O1Ai—K2—O1Bv169.44 (4)
O2Wi—K1—N9Bii83.53 (4)O1B—K2—O1Bv90.77 (4)
N3A—K1—N9Bii147.30 (4)O1A—K2—O1Bvi83.28 (4)
N3Bii—K1—N9Bii47.82 (4)O1Ai—K2—O1Bvi88.52 (4)
O2W—K1—O2Wiii83.95 (4)O1B—K2—O1Bvi86.02 (4)
O2Wi—K1—O2Wiii63.03 (4)O1Bv—K2—O1Bvi81.06 (4)
N3A—K1—O2Wiii154.43 (4)O1A—K2—O3W82.69 (4)
N3Bii—K1—O2Wiii100.94 (4)O1Ai—K2—O3W107.78 (4)
N9Bii—K1—O2Wiii56.25 (4)O1B—K2—O3W107.47 (4)
O2W—K1—N9Biv82.66 (4)O1Bv—K2—O3W82.76 (4)
O2Wi—K1—N9Biv139.63 (4)O1Bvi—K2—O3W159.05 (4)
N3A—K1—N9Biv96.67 (4)O1A—K2—C6Ai75.32 (4)
N3Bii—K1—N9Biv69.65 (4)O1Ai—K2—C6Ai21.11 (4)
N9Bii—K1—N9Biv77.61 (3)O1B—K2—C6Ai106.56 (4)
O2Wiii—K1—N9Biv76.84 (4)O1Bv—K2—C6Ai162.42 (4)
O2W—K1—N3Ai121.66 (4)O1Bvi—K2—C6Ai96.92 (4)
O2Wi—K1—N3Ai64.80 (4)O3W—K2—C6Ai94.48 (4)
N3A—K1—N3Ai77.39 (3)O1A—K2—C6Bv101.48 (4)
N3Bii—K1—N3Ai81.93 (4)O1Ai—K2—C6Bv164.89 (4)
N9Bii—K1—N3Ai91.37 (4)O1B—K2—C6Bv79.00 (4)
O2Wiii—K1—N3Ai120.29 (4)O1Bv—K2—C6Bv19.17 (3)
N9Biv—K1—N3Ai149.64 (4)O1Bvi—K2—C6Bv95.31 (4)
O2W—K1—C4Bii147.82 (4)O3W—K2—C6Bv72.42 (4)
O2Wi—K1—C4Bii104.97 (4)C6Ai—K2—C6Bv166.88 (4)
N3A—K1—C4Bii123.99 (4)O1A—K2—K2i136.12 (3)
N3Bii—K1—C4Bii24.31 (4)O1Ai—K2—K2i42.65 (2)
N9Bii—K1—C4Bii24.19 (4)O1B—K2—K2i45.04 (3)
O2Wiii—K1—C4Bii76.98 (4)O1Bv—K2—K2i135.81 (3)
N9Biv—K1—C4Bii67.98 (4)O1Bvi—K2—K2i93.53 (3)
N3Ai—K1—C4Bii90.45 (4)O3W—K2—K2i107.36 (3)
O2W—K1—C4A66.78 (4)C6Ai—K2—K2i61.58 (3)
O2Wi—K1—C4A94.15 (4)C6Bv—K2—K2i122.36 (3)
N3A—K1—C4A23.28 (4)O1A—K2—K2v43.88 (3)
N3Bii—K1—C4A115.17 (4)O1Ai—K2—K2v137.35 (3)
N9Bii—K1—C4A154.24 (4)O1B—K2—K2v134.96 (3)
O2Wiii—K1—C4A143.75 (4)O1Bv—K2—K2v44.19 (3)
N9Biv—K1—C4A117.71 (4)O1Bvi—K2—K2v86.48 (3)
N3Ai—K1—C4A64.82 (4)O3W—K2—K2v72.63 (3)
C4Bii—K1—C4A138.60 (4)C6Ai—K2—K2v118.42 (3)
O2W—K1—N9A52.52 (4)C6Bv—K2—K2v57.63 (3)
O2Wi—K1—N9A76.40 (4)K2i—K2—K2v180.0
N3A—K1—N9A43.73 (4)O1A—K2—K2vi125.81 (3)
N3Bii—K1—N9A137.43 (4)O1Ai—K2—K2vi86.75 (3)
N9Bii—K1—N9A157.24 (4)O1B—K2—K2vi43.48 (3)
O2Wiii—K1—N9A120.77 (4)O1Bv—K2—K2vi84.38 (3)
N9Biv—K1—N9A124.91 (4)O1Bvi—K2—K2vi42.53 (3)
N3Ai—K1—N9A70.51 (4)O3W—K2—K2vi147.96 (3)
C4Bii—K1—N9A158.54 (4)C6Ai—K2—K2vi106.03 (3)
C4A—K1—N9A23.14 (4)C6Bv—K2—K2vi86.25 (3)
O2W—K1—K1i133.81 (3)K2i—K2—K2vi64.121 (12)
O2Wi—K1—K1i45.15 (3)K2v—K2—K2vi115.881 (11)
N3A—K1—K1i124.58 (3)O1A—K2—K2vii83.67 (3)
N3Bii—K1—K1i75.74 (3)O1Ai—K2—K2vii128.96 (3)
N9Bii—K1—K1i52.23 (3)O1B—K2—K2vii87.88 (3)
O2Wiii—K1—K1i75.37 (3)O1Bv—K2—K2vii40.60 (3)
N9Biv—K1—K1i129.84 (3)O1Bvi—K2—K2vii40.46 (3)
N3Ai—K1—K1i47.20 (3)O3W—K2—K2vii122.17 (3)
C4Bii—K1—K1i65.56 (3)C6Ai—K2—K2vii134.88 (3)
C4A—K1—K1i109.38 (3)C6Bv—K2—K2vii55.98 (3)
N9A—K1—K1i105.17 (3)K2i—K2—K2vii120.766 (11)
O2W—K1—H516.7 (3)K2v—K2—K2vii59.237 (11)
O2Wi—K1—H583.8 (4)K2vi—K2—K2vii56.644 (12)
N3A—K1—H559.8 (4)O1A—K2—H11101.2 (3)
N3Bii—K1—H5154.9 (4)O1Ai—K2—H11105.7 (4)
N9Bii—K1—H5152.2 (4)O1B—K2—H1189.1 (3)
O2Wiii—K1—H596.0 (4)O1Bv—K2—H1184.4 (4)
N9Biv—K1—H596.7 (4)O1Bvi—K2—H11164.6 (4)
N3Ai—K1—H5105.4 (3)O3W—K2—H1118.5 (2)
C4Bii—K1—H5164.1 (3)C6Ai—K2—H1198.5 (4)
C4A—K1—H551.5 (3)C6Bv—K2—H1169.4 (4)
N9A—K1—H535.8 (3)K2i—K2—H1193.3 (3)
K1i—K1—H5127.0 (4)K2v—K2—H1186.7 (3)
N9A—C8A—N7A113.85 (17)K2vi—K2—H11130.8 (3)
N9A—C8A—H1125.4 (11)K2vii—K2—H11124.9 (4)
N7A—C8A—H1120.7 (11)N7B—C8B—N9B117.29 (15)
N3A—C4A—N9A124.90 (14)N7B—C8B—H7121.0 (11)
N3A—C4A—C5A124.72 (15)N9B—C8B—H7121.7 (11)
N9A—C4A—C5A110.37 (14)N9B—C4B—N3B124.91 (13)
N3A—C4A—K157.74 (8)N9B—C4B—C5B109.69 (14)
N9A—C4A—K180.88 (9)N3B—C4B—C5B125.39 (15)
C5A—C4A—K1139.10 (12)N9B—C4B—K1viii66.56 (8)
C4A—C5A—N7A105.64 (15)N3B—C4B—K1viii61.37 (8)
C4A—C5A—C6A120.33 (14)C5B—C4B—K1viii160.33 (11)
N7A—C5A—C6A134.01 (15)N7B—C5B—C4B108.84 (14)
O1A—C6A—N1A120.52 (15)N7B—C5B—C6B130.98 (14)
O1A—C6A—C5A124.89 (14)C4B—C5B—C6B120.15 (14)
N1A—C6A—C5A114.59 (14)O1B—C6B—N1B119.41 (15)
O1A—C6A—K2v49.64 (8)O1B—C6B—C5B128.45 (15)
N1A—C6A—K2v111.13 (10)N1B—C6B—C5B112.13 (13)
C5A—C6A—K2v109.86 (10)O1B—C6B—K2i46.05 (8)
N3A—C2A—N1A128.98 (14)N1B—C6B—K2i113.21 (10)
N3A—C2A—N2A117.39 (14)C5B—C6B—K2i112.16 (10)
N1A—C2A—N2A113.55 (15)N3B—C2B—N2B120.51 (13)
C8A—N9A—C4A103.96 (14)N3B—C2B—N1B123.62 (14)
C8A—N9A—K1140.67 (15)N2B—C2B—N1B115.82 (14)
C4A—N9A—K175.99 (9)C8B—N7B—C5B101.92 (12)
C8A—N7A—C5A106.18 (14)C8B—N9B—C4B102.24 (13)
C8A—N7A—H2126.2 (13)C8B—N9B—K1viii155.66 (11)
C5A—N7A—H2127.5 (13)C4B—N9B—K1viii89.25 (9)
C2A—N1A—C6A120.22 (14)C8B—N9B—K1ix115.02 (11)
C2A—N3A—C4A111.09 (13)C4B—N9B—K1ix115.74 (10)
C2A—N3A—K1123.85 (10)K1viii—N9B—K1ix77.60 (3)
C4A—N3A—K198.99 (10)C2B—N3B—C4B113.85 (12)
C2A—N3A—K1v114.61 (10)C2B—N3B—K1viii144.90 (10)
C4A—N3A—K1v126.59 (10)C4B—N3B—K1viii94.32 (9)
K1—N3A—K1v77.39 (3)C2B—N1B—C6B124.84 (14)
C2A—N2A—H3114.1 (13)C2B—N1B—H8116.6 (12)
C2A—N2A—H4113.9 (12)C6B—N1B—H8118.5 (12)
H3—N2A—H4114.4 (18)C2B—N2B—H9116.8 (14)
C6A—O1A—K2142.38 (11)C2B—N2B—H10117.1 (11)
C6A—O1A—K2v109.25 (10)H9—N2B—H10116.1 (18)
K2—O1A—K2v93.47 (4)C6B—O1B—K2123.86 (10)
K1—O2W—K1v88.66 (4)C6B—O1B—K2i114.77 (10)
K1—O2W—K1iii96.05 (4)K2—O1B—K2i90.77 (3)
K1v—O2W—K1iii116.97 (4)C6B—O1B—K2vi126.62 (10)
K1—O2W—H586.7 (15)K2—O1B—K2vi93.98 (4)
K1v—O2W—H5107.0 (15)K2i—O1B—K2vi98.94 (4)
K1iii—O2W—H5135.9 (15)K2—O3W—H1180.0 (14)
K1—O2W—H6157.0 (16)K2—O3W—H12104.5 (14)
K1v—O2W—H6105.3 (16)H11—O3W—H12107.5 (14)
N3A—C4A—C5A—N7A178.91 (16)N3B—C4B—C5B—N7B178.01 (15)
N9A—C4A—C5A—N7A0.2 (2)K1viii—C4B—C5B—N7B74.1 (4)
K1—C4A—C5A—N7A99.97 (18)N9B—C4B—C5B—C6B179.38 (15)
N3A—C4A—C5A—C6A0.5 (3)N3B—C4B—C5B—C6B0.1 (2)
N9A—C4A—C5A—C6A178.23 (16)K1viii—C4B—C5B—C6B104.1 (3)
K1—C4A—C5A—C6A78.4 (2)N7B—C5B—C6B—O1B0.9 (3)
C4A—C5A—C6A—O1A177.53 (16)C4B—C5B—C6B—O1B178.57 (16)
N7A—C5A—C6A—O1A0.3 (3)N7B—C5B—C6B—N1B178.49 (16)
C4A—C5A—C6A—N1A2.5 (2)C4B—C5B—C6B—N1B0.8 (2)
N7A—C5A—C6A—N1A179.62 (18)N7B—C5B—C6B—K2i49.8 (2)
C4A—C5A—C6A—K2v128.46 (15)C4B—C5B—C6B—K2i127.87 (13)
N7A—C5A—C6A—K2v53.7 (2)N9B—C8B—N7B—C5B0.5 (2)
N7A—C8A—N9A—C4A0.2 (3)C4B—C5B—N7B—C8B1.01 (18)
N7A—C8A—N9A—K184.6 (2)C6B—C5B—N7B—C8B178.89 (17)
N3A—C4A—N9A—C8A178.96 (18)N7B—C8B—N9B—C4B0.2 (2)
C5A—C4A—N9A—C8A0.2 (2)N7B—C8B—N9B—K1viii116.8 (2)
K1—C4A—N9A—C8A139.42 (15)N7B—C8B—N9B—K1ix126.06 (14)
N3A—C4A—N9A—K139.54 (16)N3B—C4B—N9B—C8B178.39 (16)
C5A—C4A—N9A—K1139.20 (15)C5B—C4B—N9B—C8B0.86 (18)
N9A—C8A—N7A—C5A0.1 (3)K1viii—C4B—N9B—C8B158.36 (13)
C4A—C5A—N7A—C8A0.0 (2)N3B—C4B—N9B—K1viii20.03 (16)
C6A—C5A—N7A—C8A178.0 (2)C5B—C4B—N9B—K1viii159.22 (12)
N3A—C2A—N1A—C6A1.3 (3)N3B—C4B—N9B—K1ix55.81 (18)
N2A—C2A—N1A—C6A175.58 (15)C5B—C4B—N9B—K1ix124.94 (11)
O1A—C6A—N1A—C2A177.20 (15)K1viii—C4B—N9B—K1ix75.84 (6)
C5A—C6A—N1A—C2A2.8 (2)N2B—C2B—N3B—C4B177.93 (14)
K2v—C6A—N1A—C2A128.12 (13)N1B—C2B—N3B—C4B0.5 (2)
N1A—C2A—N3A—C4A0.8 (3)N2B—C2B—N3B—K1viii41.5 (2)
N2A—C2A—N3A—C4A177.58 (15)N1B—C2B—N3B—K1viii141.01 (14)
N1A—C2A—N3A—K1116.56 (16)N9B—C4B—N3B—C2B179.49 (15)
N2A—C2A—N3A—K160.18 (19)C5B—C4B—N3B—C2B0.4 (2)
N1A—C2A—N3A—K1v152.41 (14)K1viii—C4B—N3B—C2B158.51 (14)
N2A—C2A—N3A—K1v30.85 (18)N9B—C4B—N3B—K1viii20.98 (16)
N9A—C4A—N3A—C2A179.73 (17)C5B—C4B—N3B—K1viii158.15 (15)
C5A—C4A—N3A—C2A1.2 (2)N3B—C2B—N1B—C6B1.6 (2)
K1—C4A—N3A—C2A131.71 (15)N2B—C2B—N1B—C6B179.17 (15)
N9A—C4A—N3A—K148.02 (19)O1B—C6B—N1B—C2B177.79 (15)
C5A—C4A—N3A—K1130.55 (16)C5B—C6B—N1B—C2B1.6 (2)
N9A—C4A—N3A—K1v32.9 (2)K2i—C6B—N1B—C2B126.48 (13)
C5A—C4A—N3A—K1v148.53 (14)N1B—C6B—O1B—K2156.01 (11)
K1—C4A—N3A—K1v80.92 (9)C5B—C6B—O1B—K224.7 (2)
N1A—C6A—O1A—K2143.31 (14)K2i—C6B—O1B—K2109.12 (12)
C5A—C6A—O1A—K236.7 (3)N1B—C6B—O1B—K2i94.87 (15)
K2v—C6A—O1A—K2123.94 (17)C5B—C6B—O1B—K2i84.46 (18)
N1A—C6A—O1A—K2v92.75 (15)N1B—C6B—O1B—K2vi28.9 (2)
C5A—C6A—O1A—K2v87.19 (17)C5B—C6B—O1B—K2vi151.74 (13)
N9B—C4B—C5B—N7B1.23 (18)K2i—C6B—O1B—K2vi123.80 (14)
Symmetry codes: (i) x, y+1, z; (ii) x+1/2, y+3/2, z+1/2; (iii) x+1, y, z+2; (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1; (vii) x+1/2, y+1/2, z+1; (viii) x1/2, y+3/2, z1/2; (ix) x1/2, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N9A0.81 (2)2.02 (2)2.8179 (19)166 (2)
N7A—H2···O3W0.871 (19)1.962 (19)2.8285 (19)172.6 (19)
O3W—H11···N7B0.95 (1)1.86 (1)2.7793 (19)165 (2)
N2A—H3···N3Biv0.862 (19)2.242 (19)3.044 (2)154.8 (17)
N1B—H8···O1Avi0.840 (18)2.155 (19)2.9893 (18)172.1 (16)
O3W—H12···N7Bv0.93 (1)2.03 (2)2.925 (2)159 (2)
Symmetry codes: (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1.
potassium{2-amino-6-oxo-1-hydro-purine-7(9)-ide/2-amino-6-oxo-7-hydro-purine-1(3)-ide}monohydrate (300K) top
Crystal data top
C10H12K2N10O4F(000) = 1696
Mr = 414.50Dx = 1.751 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 36.591 (3) ÅCell parameters from 7120 reflections
b = 3.8847 (2) Åθ = 2.8–28.0°
c = 28.759 (3) ŵ = 0.65 mm1
β = 129.719 (15)°T = 300 K
V = 3144.4 (7) Å3Needle, colourless
Z = 80.4 × 0.1 × 0.03 mm
Data collection top
Xcalibur, Ruby, Gemini ultra
diffractometer
4189 independent reflections
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source2632 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.063
Detector resolution: 10.3457 pixels mm-1θmax = 29.5°, θmin = 2.2°
ω scansh = 5049
Absorption correction: multi-scan
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 55
Tmin = 0.833, Tmax = 1.000l = 3937
26811 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: difference Fourier map
wR(F2) = 0.077Only H-atom coordinates refined
S = 0.87 w = 1/[σ2(Fo2) + (0.041P)2]
where P = (Fo2 + 2Fc2)/3
4189 reflections(Δ/σ)max = 0.001
271 parametersΔρmax = 0.31 e Å3
3 restraintsΔρmin = 0.29 e Å3
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*/Ueq
K10.49288 (2)0.14562 (12)0.92182 (2)0.03421 (12)
C8A0.33165 (7)0.0501 (7)0.79376 (9)0.0466 (6)
H10.3119 (8)0.114 (6)0.8049 (9)0.056*
C4A0.38665 (6)0.1435 (5)0.79536 (7)0.0263 (4)
C5A0.35046 (5)0.0387 (5)0.73685 (7)0.0261 (4)
C6A0.35562 (5)0.0648 (4)0.69244 (7)0.0227 (4)
C2A0.42993 (5)0.3030 (4)0.76998 (7)0.0215 (4)
N9A0.37445 (5)0.0865 (5)0.83115 (7)0.0395 (4)
N7A0.31539 (5)0.0860 (5)0.73722 (7)0.0361 (4)
H20.2878 (7)0.164 (5)0.7068 (9)0.043*
N1A0.39680 (4)0.2091 (4)0.71169 (6)0.0239 (3)
N3A0.42856 (4)0.2793 (4)0.81485 (6)0.0254 (3)
N2A0.47122 (5)0.4243 (4)0.78391 (7)0.0290 (4)
H30.4896 (7)0.523 (5)0.8185 (9)0.035*
H40.4674 (6)0.534 (5)0.7550 (9)0.035*
O1A0.32507 (4)0.0369 (3)0.63803 (5)0.0286 (3)
O2W0.45245 (4)0.3458 (4)0.94549 (6)0.0363 (3)
H50.4267 (6)0.300 (6)0.9129 (8)0.044*
H60.4452 (7)0.435 (6)0.9640 (9)0.044*
K20.26246 (2)0.52594 (10)0.57129 (2)0.03006 (12)
C8B0.11975 (6)0.7425 (5)0.54155 (8)0.0296 (4)
H70.1216 (6)0.648 (5)0.5722 (9)0.036*
C4B0.09142 (5)1.0006 (4)0.46020 (7)0.0201 (3)
C5B0.13928 (5)0.9363 (4)0.49159 (7)0.0211 (4)
C6B0.16115 (5)1.0479 (4)0.46800 (7)0.0208 (4)
C2B0.08238 (5)1.2701 (4)0.38443 (7)0.0198 (4)
N7B0.15784 (5)0.7709 (4)0.54532 (6)0.0274 (3)
N9B0.07847 (5)0.8742 (4)0.49186 (6)0.0254 (3)
N3B0.06163 (4)1.1684 (4)0.40606 (6)0.0208 (3)
N1B0.12942 (4)1.2114 (4)0.41278 (6)0.0218 (3)
H80.1392 (6)1.289 (5)0.3959 (8)0.026*
N2B0.05720 (5)1.4302 (4)0.33032 (7)0.0268 (4)
H90.0326 (7)1.522 (5)0.3177 (9)0.032*
H100.0740 (6)1.536 (5)0.3214 (8)0.032*
O1B0.20352 (4)1.0182 (3)0.49051 (5)0.0286 (3)
O3W0.22480 (4)0.3000 (4)0.63164 (6)0.0496 (4)
H110.2045 (7)0.483 (3)0.6075 (10)0.060*
H120.2091 (7)0.095 (3)0.6135 (10)0.060*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0364 (2)0.0364 (2)0.0358 (2)0.00874 (18)0.0259 (2)0.00588 (19)
C8A0.0349 (11)0.0752 (17)0.0352 (12)0.0157 (11)0.0249 (10)0.0053 (11)
C4A0.0230 (8)0.0329 (10)0.0196 (8)0.0003 (7)0.0120 (7)0.0013 (8)
C5A0.0197 (8)0.0336 (11)0.0215 (9)0.0023 (7)0.0116 (7)0.0020 (7)
C6A0.0187 (8)0.0238 (10)0.0189 (9)0.0042 (6)0.0090 (7)0.0009 (7)
C2A0.0192 (8)0.0221 (9)0.0199 (8)0.0021 (7)0.0109 (7)0.0002 (7)
N9A0.0326 (8)0.0634 (12)0.0248 (8)0.0147 (8)0.0194 (7)0.0084 (8)
N7A0.0248 (8)0.0554 (12)0.0256 (9)0.0137 (7)0.0149 (7)0.0075 (8)
N1A0.0205 (7)0.0297 (8)0.0190 (7)0.0005 (6)0.0115 (6)0.0023 (6)
N3A0.0209 (7)0.0339 (9)0.0183 (7)0.0029 (6)0.0111 (6)0.0022 (6)
N2A0.0220 (7)0.0418 (10)0.0207 (8)0.0072 (7)0.0124 (7)0.0044 (7)
O1A0.0234 (6)0.0353 (7)0.0168 (6)0.0030 (5)0.0080 (5)0.0057 (5)
O2W0.0280 (7)0.0526 (9)0.0276 (7)0.0005 (6)0.0174 (6)0.0099 (7)
K20.0266 (2)0.0296 (2)0.0280 (2)0.00176 (16)0.01464 (18)0.00339 (17)
C8B0.0321 (10)0.0329 (11)0.0259 (10)0.0003 (8)0.0195 (9)0.0048 (8)
C4B0.0213 (8)0.0213 (9)0.0189 (8)0.0017 (7)0.0134 (7)0.0030 (7)
C5B0.0188 (8)0.0230 (9)0.0184 (8)0.0002 (6)0.0105 (7)0.0002 (7)
C6B0.0181 (8)0.0214 (9)0.0201 (8)0.0012 (6)0.0109 (7)0.0036 (7)
C2B0.0178 (8)0.0208 (9)0.0182 (8)0.0012 (6)0.0103 (7)0.0036 (7)
N7B0.0252 (7)0.0314 (9)0.0226 (8)0.0028 (6)0.0139 (6)0.0056 (6)
N9B0.0247 (7)0.0312 (9)0.0239 (8)0.0003 (6)0.0172 (7)0.0020 (6)
N3B0.0175 (6)0.0273 (8)0.0188 (7)0.0000 (6)0.0121 (6)0.0003 (6)
N1B0.0184 (7)0.0299 (9)0.0190 (7)0.0001 (6)0.0128 (6)0.0026 (6)
N2B0.0187 (7)0.0373 (10)0.0251 (8)0.0059 (6)0.0142 (7)0.0104 (7)
O1B0.0154 (6)0.0403 (8)0.0261 (7)0.0031 (5)0.0115 (5)0.0041 (6)
O3W0.0300 (7)0.0462 (10)0.0404 (9)0.0058 (6)0.0075 (6)0.0058 (7)
Geometric parameters (Å, º) top
K1—O2W2.7538 (15)O1A—K2v2.6931 (13)
K1—O2Wi2.8004 (16)O2W—H50.819 (16)
K1—N3A2.9110 (16)O2W—H60.808 (17)
K1—N3Bii2.9178 (14)K2—O1B2.7022 (13)
K1—N9Bii3.0469 (16)K2—O1Bv2.7449 (14)
K1—O2Wiii3.0678 (16)K2—O1Bvi2.7508 (13)
K1—N9Biv3.1435 (15)K2—O3W2.9559 (18)
K1—N3Ai3.2771 (15)K2—C6Bv3.4555 (17)
K1—C4Bii3.3201 (17)K2—K2i3.8847 (2)
K1—C4A3.3956 (19)K2—K2v3.8847 (2)
K1—N9A3.4567 (18)K2—K2vi3.9874 (9)
K1—K1v3.8846 (2)K2—K2vii4.1791 (9)
K1—H52.85 (2)K2—H112.90 (2)
C8A—N9A1.318 (3)C8B—N7B1.332 (2)
C8A—N7A1.335 (3)C8B—N9B1.351 (2)
C8A—H10.99 (2)C8B—H70.92 (2)
C4A—N3A1.359 (2)C4B—N9B1.359 (2)
C4A—N9A1.377 (2)C4B—N3B1.367 (2)
C4A—C5A1.379 (2)C4B—C5B1.387 (2)
C5A—N7A1.378 (2)C5B—N7B1.386 (2)
C5A—C6A1.409 (2)C5B—C6B1.408 (2)
C6A—O1A1.2722 (19)C6B—O1B1.2465 (19)
C6A—N1A1.351 (2)C6B—N1B1.384 (2)
C6A—K2v3.3328 (17)C2B—N3B1.313 (2)
C2A—N3A1.326 (2)C2B—N2B1.351 (2)
C2A—N1A1.347 (2)C2B—N1B1.373 (2)
C2A—N2A1.376 (2)N1B—H80.821 (19)
N7A—H20.86 (2)N2B—H90.809 (19)
N2A—H30.86 (2)N2B—H100.90 (2)
N2A—H40.86 (2)O3W—H110.938 (13)
O1A—K22.6310 (12)O3W—H120.925 (13)
O2W—K1—O2Wi88.75 (4)K1iii—O2W—H661.1 (16)
O2W—K1—N3A70.67 (4)H5—O2W—H6103 (2)
O2Wi—K1—N3A117.45 (4)O1A—K2—O1Ai93.71 (4)
O2W—K1—N3Bii149.63 (5)O1A—K2—O1B169.33 (4)
O2Wi—K1—N3Bii120.33 (5)O1Ai—K2—O1B86.51 (4)
N3A—K1—N3Bii99.86 (4)O1A—K2—O1Bv86.88 (4)
O2W—K1—N9Bii138.47 (4)O1Ai—K2—O1Bv169.48 (4)
O2Wi—K1—N9Bii83.51 (4)O1B—K2—O1Bv90.98 (4)
N3A—K1—N9Bii147.25 (4)O1A—K2—O1Bvi83.32 (4)
N3Bii—K1—N9Bii47.70 (4)O1Ai—K2—O1Bvi88.64 (4)
O2W—K1—O2Wiii83.95 (4)O1B—K2—O1Bvi86.02 (4)
O2Wi—K1—O2Wiii62.91 (5)O1Bv—K2—O1Bvi80.99 (4)
N3A—K1—O2Wiii154.48 (4)O1A—K2—O3W82.68 (4)
N3Bii—K1—O2Wiii100.88 (4)O1Ai—K2—O3W107.69 (4)
N9Bii—K1—O2Wiii56.27 (4)O1B—K2—O3W107.43 (4)
O2W—K1—N9Biv82.47 (4)O1Bv—K2—O3W82.80 (4)
O2Wi—K1—N9Biv139.66 (4)O1Bvi—K2—O3W159.09 (5)
N3A—K1—N9Biv96.57 (4)O1A—K2—C6Ai75.50 (4)
N3Bii—K1—N9Biv69.74 (4)O1Ai—K2—C6Ai21.15 (4)
N9Bii—K1—N9Biv77.72 (3)O1B—K2—C6Ai106.40 (4)
O2Wiii—K1—N9Biv77.00 (4)O1Bv—K2—C6Ai162.38 (4)
O2W—K1—N3Ai121.85 (4)O1Bvi—K2—C6Ai97.03 (4)
O2Wi—K1—N3Ai64.74 (4)O3W—K2—C6Ai94.41 (4)
N3A—K1—N3Ai77.52 (3)O1A—K2—C6Bv101.23 (4)
N3Bii—K1—N3Ai81.87 (4)O1Ai—K2—C6Bv164.90 (4)
N9Bii—K1—N3Ai91.23 (4)O1B—K2—C6Bv79.22 (4)
O2Wiii—K1—N3Ai120.07 (4)O1Bv—K2—C6Bv19.14 (4)
N9Biv—K1—N3Ai149.67 (4)O1Bvi—K2—C6Bv95.21 (4)
O2W—K1—C4Bii147.74 (4)O3W—K2—C6Bv72.47 (4)
O2Wi—K1—C4Bii104.91 (4)C6Ai—K2—C6Bv166.85 (4)
N3A—K1—C4Bii123.98 (4)O1A—K2—K2i136.23 (3)
N3Bii—K1—C4Bii24.23 (4)O1Ai—K2—K2i42.52 (3)
N9Bii—K1—C4Bii24.15 (4)O1B—K2—K2i44.95 (3)
O2Wiii—K1—C4Bii77.00 (4)O1Bv—K2—K2i135.93 (3)
N9Biv—K1—C4Bii68.11 (4)O1Bvi—K2—K2i93.58 (3)
N3Ai—K1—C4Bii90.33 (4)O3W—K2—K2i107.27 (3)
O2W—K1—C4A66.88 (4)C6Ai—K2—K2i61.51 (3)
O2Wi—K1—C4A94.17 (4)C6Bv—K2—K2i122.50 (3)
N3A—K1—C4A23.29 (4)O1A—K2—K2v43.77 (3)
N3Bii—K1—C4A115.21 (4)O1Ai—K2—K2v137.48 (3)
N9Bii—K1—C4A154.17 (4)O1B—K2—K2v135.05 (3)
O2Wiii—K1—C4A143.74 (4)O1Bv—K2—K2v44.07 (3)
N9Biv—K1—C4A117.63 (5)O1Bvi—K2—K2v86.42 (3)
N3Ai—K1—C4A64.92 (4)O3W—K2—K2v72.73 (3)
C4Bii—K1—C4A138.57 (4)C6Ai—K2—K2v118.49 (3)
O2W—K1—N9A52.64 (4)C6Bv—K2—K2v57.49 (3)
O2Wi—K1—N9A76.41 (4)K2i—K2—K2v180.0
N3A—K1—N9A43.76 (4)O1A—K2—K2vi125.85 (3)
N3Bii—K1—N9A137.48 (4)O1Ai—K2—K2vi86.70 (3)
N9Bii—K1—N9A157.20 (4)O1B—K2—K2vi43.49 (3)
O2Wiii—K1—N9A120.74 (4)O1Bv—K2—K2vi84.47 (3)
N9Biv—K1—N9A124.84 (5)O1Bvi—K2—K2vi42.54 (3)
N3Ai—K1—N9A70.59 (4)O3W—K2—K2vi147.94 (3)
C4Bii—K1—N9A158.50 (4)C6Ai—K2—K2vi106.01 (4)
C4A—K1—N9A23.16 (4)C6Bv—K2—K2vi86.32 (3)
O2W—K1—K1v46.11 (3)K2i—K2—K2vi64.113 (12)
O2Wi—K1—K1v134.87 (3)K2v—K2—K2vi115.885 (12)
N3A—K1—K1v55.46 (3)O1A—K2—K2vii83.55 (3)
N3Bii—K1—K1v104.34 (3)O1Ai—K2—K2vii129.06 (3)
N9Bii—K1—K1v127.75 (3)O1B—K2—K2vii88.03 (3)
O2Wiii—K1—K1v104.69 (3)O1Bv—K2—K2vii40.55 (3)
N9Biv—K1—K1v50.03 (3)O1Bvi—K2—K2vii40.44 (3)
N3Ai—K1—K1v132.97 (3)O3W—K2—K2vii122.18 (4)
C4Bii—K1—K1v114.46 (3)C6Ai—K2—K2vii134.95 (3)
C4A—K1—K1v70.68 (3)C6Bv—K2—K2vii55.89 (3)
N9A—K1—K1v74.88 (3)K2i—K2—K2vii120.862 (11)
O2W—K1—H516.7 (3)K2v—K2—K2vii59.136 (12)
O2Wi—K1—H584.3 (4)K2vi—K2—K2vii56.749 (13)
N3A—K1—H559.6 (4)O1A—K2—H11101.1 (3)
N3Bii—K1—H5154.6 (5)O1Ai—K2—H11105.7 (4)
N9Bii—K1—H5152.4 (4)O1B—K2—H1189.1 (3)
O2Wiii—K1—H596.2 (4)O1Bv—K2—H1184.5 (4)
N9Biv—K1—H596.2 (4)O1Bvi—K2—H11164.6 (4)
N3Ai—K1—H5105.7 (4)O3W—K2—H1118.4 (2)
C4Bii—K1—H5163.9 (4)C6Ai—K2—H1198.4 (4)
C4A—K1—H551.5 (4)C6Bv—K2—H1169.5 (4)
N9A—K1—H536.0 (3)K2i—K2—H1193.3 (3)
K1v—K1—H552.6 (4)K2v—K2—H1186.7 (3)
N9A—C8A—N7A114.09 (19)K2vi—K2—H11130.9 (3)
N9A—C8A—H1124.7 (12)K2vii—K2—H11124.8 (4)
N7A—C8A—H1121.2 (12)N7B—C8B—N9B117.33 (16)
N3A—C4A—N9A125.02 (15)N7B—C8B—H7121.7 (12)
N3A—C4A—C5A124.64 (16)N9B—C8B—H7120.9 (12)
N9A—C4A—C5A110.34 (15)N9B—C4B—N3B124.74 (14)
N3A—C4A—K157.91 (9)N9B—C4B—C5B109.57 (14)
N9A—C4A—K180.91 (10)N3B—C4B—C5B125.68 (15)
C5A—C4A—K1139.33 (13)N9B—C4B—K1viii66.58 (9)
N7A—C5A—C4A105.49 (15)N3B—C4B—K1viii61.17 (8)
N7A—C5A—C6A134.19 (16)C5B—C4B—K1viii160.44 (12)
C4A—C5A—C6A120.29 (15)N7B—C5B—C4B108.92 (15)
O1A—C6A—N1A120.41 (16)N7B—C5B—C6B130.97 (14)
O1A—C6A—C5A124.83 (15)C4B—C5B—C6B120.07 (15)
N1A—C6A—C5A114.75 (14)O1B—C6B—N1B119.42 (16)
O1A—C6A—K2v49.80 (8)O1B—C6B—C5B128.50 (15)
N1A—C6A—K2v111.00 (11)N1B—C6B—C5B112.08 (14)
C5A—C6A—K2v110.00 (10)O1B—C6B—K2i46.22 (8)
N3A—C2A—N1A128.93 (15)N1B—C6B—K2i113.08 (10)
N3A—C2A—N2A117.25 (14)C5B—C6B—K2i112.27 (10)
N1A—C2A—N2A113.74 (16)N3B—C2B—N2B120.59 (14)
C8A—N9A—C4A103.81 (15)N3B—C2B—N1B123.62 (15)
C8A—N9A—K1140.68 (16)N2B—C2B—N1B115.73 (15)
C4A—N9A—K175.93 (10)C8B—N7B—C5B101.89 (13)
C8A—N7A—C5A106.28 (15)C8B—N9B—C4B102.27 (14)
C8A—N7A—H2126.2 (14)C8B—N9B—K1viii155.89 (12)
C5A—N7A—H2127.4 (14)C4B—N9B—K1viii89.27 (9)
C2A—N1A—C6A120.23 (15)C8B—N9B—K1ix114.66 (12)
C2A—N3A—C4A111.10 (14)C4B—N9B—K1ix115.73 (10)
C2A—N3A—K1124.06 (11)K1viii—N9B—K1ix77.72 (3)
C4A—N3A—K198.80 (11)C2B—N3B—C4B113.68 (13)
C2A—N3A—K1v114.52 (10)C2B—N3B—K1viii144.72 (11)
C4A—N3A—K1v126.59 (11)C4B—N3B—K1viii94.60 (9)
K1—N3A—K1v77.52 (3)C2B—N1B—C6B124.84 (15)
C2A—N2A—H3113.1 (13)C2B—N1B—H8116.2 (12)
C2A—N2A—H4114.6 (12)C6B—N1B—H8118.9 (12)
H3—N2A—H4115.0 (19)C2B—N2B—H9117.6 (14)
C6A—O1A—K2142.43 (11)C2B—N2B—H10116.8 (12)
C6A—O1A—K2v109.05 (10)H9—N2B—H10115.9 (19)
K2—O1A—K2v93.70 (4)C6B—O1B—K2123.81 (11)
K1—O2W—K1v88.76 (4)C6B—O1B—K2i114.64 (11)
K1—O2W—K1iii96.05 (4)K2—O1B—K2i90.98 (4)
K1v—O2W—K1iii117.08 (5)C6B—O1B—K2vi126.62 (11)
K1—O2W—H588.5 (16)K2—O1B—K2vi93.98 (4)
K1v—O2W—H5105.9 (16)K2i—O1B—K2vi99.01 (4)
K1iii—O2W—H5136.8 (15)K2—O3W—H1177.6 (15)
K1—O2W—H6155.9 (17)K2—O3W—H12106.2 (16)
K1v—O2W—H6107.8 (17)H11—O3W—H12108.9 (15)
N3A—C4A—C5A—N7A179.07 (18)N3B—C4B—C5B—N7B178.07 (16)
N9A—C4A—C5A—N7A0.1 (2)K1viii—C4B—C5B—N7B73.7 (4)
K1—C4A—C5A—N7A99.83 (19)N9B—C4B—C5B—C6B179.17 (15)
N3A—C4A—C5A—C6A0.8 (3)N3B—C4B—C5B—C6B0.1 (3)
N9A—C4A—C5A—C6A178.42 (17)K1viii—C4B—C5B—C6B104.2 (4)
K1—C4A—C5A—C6A78.5 (2)N7B—C5B—C6B—O1B1.1 (3)
N7A—C5A—C6A—O1A0.5 (3)C4B—C5B—C6B—O1B178.49 (17)
C4A—C5A—C6A—O1A177.18 (17)N7B—C5B—C6B—N1B178.46 (17)
N7A—C5A—C6A—N1A179.8 (2)C4B—C5B—C6B—N1B1.1 (2)
C4A—C5A—C6A—N1A2.5 (3)N7B—C5B—C6B—K2i49.9 (2)
N7A—C5A—C6A—K2v53.8 (3)C4B—C5B—C6B—K2i127.50 (14)
C4A—C5A—C6A—K2v128.52 (15)N9B—C8B—N7B—C5B0.8 (2)
N7A—C8A—N9A—C4A0.1 (3)C4B—C5B—N7B—C8B1.19 (19)
N7A—C8A—N9A—K184.4 (3)C6B—C5B—N7B—C8B178.81 (18)
N3A—C4A—N9A—C8A179.2 (2)N7B—C8B—N9B—C4B0.1 (2)
C5A—C4A—N9A—C8A0.0 (2)N7B—C8B—N9B—K1viii116.9 (3)
K1—C4A—N9A—C8A139.43 (17)N7B—C8B—N9B—K1ix126.15 (15)
N3A—C4A—N9A—K139.74 (17)N3B—C4B—N9B—C8B178.61 (16)
C5A—C4A—N9A—K1139.46 (16)C5B—C4B—N9B—C8B0.71 (19)
N9A—C8A—N7A—C5A0.2 (3)K1viii—C4B—N9B—C8B158.66 (13)
C4A—C5A—N7A—C8A0.2 (2)N3B—C4B—N9B—K1viii19.96 (16)
C6A—C5A—N7A—C8A178.1 (2)C5B—C4B—N9B—K1viii159.37 (12)
N3A—C2A—N1A—C6A0.9 (3)N3B—C4B—N9B—K1ix56.02 (19)
N2A—C2A—N1A—C6A175.80 (15)C5B—C4B—N9B—K1ix124.65 (12)
O1A—C6A—N1A—C2A177.15 (15)K1viii—C4B—N9B—K1ix75.98 (7)
C5A—C6A—N1A—C2A2.6 (2)N2B—C2B—N3B—C4B177.92 (15)
K2v—C6A—N1A—C2A128.04 (13)N1B—C2B—N3B—C4B0.7 (2)
N1A—C2A—N3A—C4A0.9 (3)N2B—C2B—N3B—K1viii41.6 (3)
N2A—C2A—N3A—C4A177.53 (15)N1B—C2B—N3B—K1viii141.19 (14)
N1A—C2A—N3A—K1116.38 (17)N9B—C4B—N3B—C2B179.31 (16)
N2A—C2A—N3A—K160.2 (2)C5B—C4B—N3B—C2B0.1 (2)
N1A—C2A—N3A—K1v152.38 (15)K1viii—C4B—N3B—C2B158.37 (15)
N2A—C2A—N3A—K1v31.02 (19)N9B—C4B—N3B—K1viii20.95 (17)
N9A—C4A—N3A—C2A179.98 (18)C5B—C4B—N3B—K1viii158.27 (15)
C5A—C4A—N3A—C2A0.9 (3)N3B—C2B—N1B—C6B1.9 (3)
K1—C4A—N3A—C2A131.85 (16)N2B—C2B—N1B—C6B179.19 (16)
N9A—C4A—N3A—K148.2 (2)O1B—C6B—N1B—C2B177.70 (16)
C5A—C4A—N3A—K1130.91 (17)C5B—C6B—N1B—C2B1.9 (2)
N9A—C4A—N3A—K1v32.8 (3)K2i—C6B—N1B—C2B126.24 (14)
C5A—C4A—N3A—K1v148.15 (15)N1B—C6B—O1B—K2155.97 (11)
K1—C4A—N3A—K1v80.94 (10)C5B—C6B—O1B—K224.5 (2)
N1A—C6A—O1A—K2143.12 (14)K2i—C6B—O1B—K2109.26 (12)
C5A—C6A—O1A—K236.6 (3)N1B—C6B—O1B—K2i94.76 (15)
K2v—C6A—O1A—K2124.12 (18)C5B—C6B—O1B—K2i84.75 (19)
N1A—C6A—O1A—K2v92.76 (15)N1B—C6B—O1B—K2vi29.0 (2)
C5A—C6A—O1A—K2v87.56 (18)C5B—C6B—O1B—K2vi151.51 (14)
N9B—C4B—C5B—N7B1.25 (19)K2i—C6B—O1B—K2vi123.74 (14)
Symmetry codes: (i) x, y+1, z; (ii) x+1/2, y+3/2, z+1/2; (iii) x+1, y, z+2; (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1; (vii) x+1/2, y+1/2, z+1; (viii) x1/2, y+3/2, z1/2; (ix) x1/2, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N9A0.82 (2)2.03 (2)2.825 (2)163 (2)
N7A—H2···O3W0.86 (2)1.97 (2)2.835 (2)173 (2)
O3W—H11···N7B0.94 (1)1.86 (2)2.782 (2)167 (2)
N2A—H3···N3Biv0.86 (2)2.26 (2)3.055 (2)153.6 (18)
N1B—H8···O1Avi0.821 (19)2.181 (19)2.9957 (19)171.7 (17)
O3W—H12···N7Bv0.93 (1)2.06 (2)2.935 (2)157 (2)
Symmetry codes: (iv) x+1/2, y+1/2, z+1/2; (v) x, y1, z; (vi) x+1/2, y+3/2, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_100K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.586 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5290 (2) ÅCell parameters from 6267 reflections
b = 11.6677 (2) Åθ = 2.6–29.6°
c = 11.1762 (3) ŵ = 0.20 mm1
β = 101.608 (2)°T = 100 K
V = 1344.90 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3768 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3079 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.053
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.832, Tmax = 1.000l = 1513
12423 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: difference Fourier map
wR(F2) = 0.087Only H-atom coordinates refined
S = 1.09 w = 1/[σ2(Fo2) + (0.0365P)2 + 0.7432P]
where P = (Fo2 + 2Fc2)/3
3768 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.50 e Å3
0 restraintsΔρmin = 0.25 e Å3
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*/Ueq
N10.65496 (10)0.48310 (8)0.34808 (10)0.0110 (2)
C20.52571 (12)0.48348 (10)0.33921 (11)0.0109 (2)
N30.45233 (10)0.40271 (8)0.37681 (10)0.0112 (2)
C40.52332 (11)0.31348 (9)0.43279 (11)0.0100 (2)
C50.65758 (11)0.30531 (9)0.44965 (11)0.0105 (2)
C60.72600 (11)0.39407 (9)0.40459 (11)0.0099 (2)
N70.69782 (10)0.20358 (8)0.50960 (10)0.0121 (2)
C80.58566 (12)0.15761 (10)0.52392 (12)0.0133 (2)
H10.5849 (16)0.0874 (14)0.5631 (15)0.016*
N90.47618 (10)0.21804 (8)0.47990 (10)0.0119 (2)
N20.46125 (11)0.57534 (9)0.27861 (11)0.0164 (2)
H20.3814 (17)0.5867 (15)0.2876 (16)0.020*
H30.5109 (17)0.6356 (15)0.2731 (16)0.020*
O10.85035 (8)0.39330 (7)0.41334 (8)0.01105 (17)
Na10.11557 (5)0.25426 (4)0.18372 (5)0.01081 (11)
Na20.04857 (5)0.04504 (4)0.37262 (5)0.01089 (11)
O2W0.30720 (9)0.32585 (8)0.13623 (9)0.01338 (18)
H40.3522 (17)0.3073 (14)0.0916 (17)0.016*
H50.3589 (17)0.3415 (14)0.2032 (17)0.016*
O3W0.18420 (9)0.38032 (7)0.35539 (9)0.01291 (18)
H60.1464 (17)0.4409 (15)0.3520 (16)0.015*
H70.2636 (18)0.3946 (14)0.3715 (16)0.015*
O4W0.24325 (9)0.11497 (7)0.32009 (9)0.01206 (17)
H80.2777 (16)0.0757 (14)0.2756 (16)0.014*
H90.3047 (17)0.1412 (15)0.3662 (16)0.014*
O5W0.00212 (9)0.06863 (7)0.14533 (8)0.01141 (17)
H100.0506 (17)0.0220 (15)0.1284 (15)0.014*
H110.0502 (17)0.0878 (14)0.0820 (17)0.014*
O6W0.15486 (9)0.02106 (8)0.42389 (9)0.01343 (18)
H120.2067 (17)0.0317 (15)0.4082 (15)0.016*
H130.1992 (17)0.0773 (15)0.4401 (16)0.016*
O7W0.04304 (9)0.22700 (7)0.46327 (8)0.01232 (18)
H140.0266 (18)0.2641 (14)0.4469 (16)0.015*
H150.0924 (17)0.2696 (15)0.4383 (16)0.015*
O8W0.08256 (9)0.14985 (7)0.31503 (9)0.01099 (17)
H160.1074 (16)0.1450 (14)0.2515 (16)0.013*
H170.1461 (17)0.1732 (14)0.3665 (16)0.013*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0107 (5)0.0112 (4)0.0113 (5)0.0013 (3)0.0025 (4)0.0009 (4)
C20.0114 (6)0.0118 (5)0.0095 (5)0.0005 (4)0.0020 (4)0.0000 (4)
N30.0088 (5)0.0133 (4)0.0113 (5)0.0012 (3)0.0014 (4)0.0005 (4)
C40.0088 (5)0.0123 (5)0.0088 (5)0.0010 (4)0.0021 (4)0.0011 (4)
C50.0076 (5)0.0112 (5)0.0128 (6)0.0006 (4)0.0020 (4)0.0014 (4)
C60.0091 (5)0.0117 (5)0.0092 (5)0.0004 (4)0.0020 (4)0.0009 (4)
N70.0114 (5)0.0117 (4)0.0129 (5)0.0014 (4)0.0016 (4)0.0021 (4)
C80.0118 (6)0.0132 (5)0.0147 (6)0.0004 (4)0.0026 (4)0.0018 (4)
N90.0099 (5)0.0128 (4)0.0132 (5)0.0001 (3)0.0030 (4)0.0014 (4)
N20.0117 (5)0.0147 (5)0.0232 (6)0.0024 (4)0.0040 (4)0.0066 (4)
O10.0070 (4)0.0146 (4)0.0118 (4)0.0011 (3)0.0025 (3)0.0008 (3)
Na10.0103 (2)0.0103 (2)0.0119 (2)0.00042 (16)0.00256 (18)0.00018 (17)
Na20.0115 (2)0.0102 (2)0.0115 (2)0.00003 (16)0.00352 (19)0.00020 (17)
O2W0.0108 (4)0.0175 (4)0.0125 (5)0.0006 (3)0.0038 (3)0.0022 (3)
O3W0.0090 (4)0.0112 (4)0.0190 (5)0.0005 (3)0.0039 (3)0.0012 (3)
O4W0.0101 (4)0.0131 (4)0.0132 (5)0.0002 (3)0.0030 (3)0.0033 (3)
O5W0.0115 (4)0.0111 (4)0.0112 (4)0.0020 (3)0.0011 (3)0.0004 (3)
O6W0.0116 (4)0.0119 (4)0.0177 (5)0.0007 (3)0.0049 (3)0.0023 (3)
O7W0.0121 (4)0.0106 (4)0.0151 (5)0.0013 (3)0.0049 (3)0.0010 (3)
O8W0.0099 (4)0.0137 (4)0.0093 (4)0.0008 (3)0.0018 (3)0.0016 (3)
Geometric parameters (Å, º) top
N1—C21.3445 (15)Na1—Na2ii4.1331 (7)
N1—C61.3592 (15)Na2—O6W2.3427 (10)
C2—N31.3388 (14)Na2—O7W2.3581 (9)
C2—N21.3722 (16)Na2—O4W2.3867 (10)
N3—C41.3587 (15)Na2—O8W2.4095 (9)
C4—N91.3670 (14)Na2—O6Wiii2.4485 (11)
C4—C51.3913 (16)Na2—O5W2.5035 (11)
C5—N71.3867 (15)Na2—Na2iii3.3807 (9)
C5—C61.4111 (15)O2W—H40.785 (18)
C6—O11.2931 (14)O2W—H50.852 (19)
N7—C81.3356 (15)O3W—H60.809 (18)
C8—N91.3563 (16)O3W—H70.836 (18)
C8—H10.930 (17)O4W—H80.813 (18)
N2—H20.877 (18)O4W—H90.802 (19)
N2—H30.886 (18)O5W—H100.826 (18)
Na1—O2W2.3413 (10)O5W—H110.814 (18)
Na1—O8Wi2.3697 (10)O6W—H120.818 (18)
Na1—O3W2.4101 (10)O6W—H130.845 (18)
Na1—O7Wii2.4380 (11)O7W—H140.839 (18)
Na1—O4W2.4386 (10)O7W—H150.808 (18)
Na1—O5W2.4892 (10)O8W—H160.807 (18)
Na1—Na23.3931 (6)O8W—H170.836 (18)
Na1—Na2i3.8021 (6)
C2—N1—C6119.41 (10)O4W—Na2—O5W74.40 (3)
N3—C2—N1127.88 (11)O8W—Na2—O5W81.11 (3)
N3—C2—N2116.45 (11)O6Wiii—Na2—O5W160.28 (4)
N1—C2—N2115.58 (10)O6W—Na2—Na2iii46.41 (3)
C2—N3—C4112.66 (10)O7W—Na2—Na2iii83.12 (3)
N3—C4—N9126.36 (11)O4W—Na2—Na2iii137.21 (4)
N3—C4—C5124.38 (10)O8W—Na2—Na2iii91.03 (3)
N9—C4—C5109.26 (10)O6Wiii—Na2—Na2iii43.86 (2)
N7—C5—C4109.11 (10)O5W—Na2—Na2iii148.20 (3)
N7—C5—C6132.25 (11)O6W—Na2—Na1123.56 (3)
C4—C5—C6118.63 (11)O7W—Na2—Na169.26 (2)
O1—C6—N1119.64 (10)O4W—Na2—Na145.94 (2)
O1—C6—C5123.35 (11)O8W—Na2—Na1116.88 (3)
N1—C6—C5117.00 (10)O6Wiii—Na2—Na1133.72 (3)
C8—N7—C5102.13 (10)O5W—Na2—Na147.01 (2)
N7—C8—N9117.08 (11)Na2iii—Na2—Na1152.09 (2)
N7—C8—H1120.1 (10)O6W—Na2—Na1iv61.74 (3)
N9—C8—H1122.8 (10)O7W—Na2—Na1iv145.57 (3)
C8—N9—C4102.43 (10)O4W—Na2—Na1iv130.43 (3)
C2—N2—H2116.8 (12)O8W—Na2—Na1iv36.93 (2)
C2—N2—H3114.5 (12)O6Wiii—Na2—Na1iv88.87 (3)
H2—N2—H3118.8 (16)O5W—Na2—Na1iv86.16 (2)
O2W—Na1—O8Wi129.25 (4)Na2iii—Na2—Na1iv69.977 (16)
O2W—Na1—O3W80.14 (3)Na1—Na2—Na1iv133.109 (15)
O8Wi—Na1—O3W80.24 (3)O6W—Na2—Na1v82.62 (3)
O2W—Na1—O7Wii81.25 (4)O7W—Na2—Na1v31.05 (2)
O8Wi—Na1—O7Wii82.33 (3)O4W—Na2—Na1v90.21 (3)
O3W—Na1—O7Wii137.10 (4)O8W—Na2—Na1v138.59 (3)
O2W—Na1—O4W89.29 (3)O6Wiii—Na2—Na1v55.14 (2)
O8Wi—Na1—O4W133.33 (4)O5W—Na2—Na1v139.17 (3)
O3W—Na1—O4W82.53 (4)Na2iii—Na2—Na1v59.804 (15)
O7Wii—Na1—O4W135.44 (4)Na1—Na2—Na1v95.402 (11)
O2W—Na1—O5W133.88 (4)Na1iv—Na2—Na1v129.780 (14)
O8Wi—Na1—O5W90.20 (3)Na1—O2W—H4134.7 (12)
O3W—Na1—O5W136.66 (4)Na1—O2W—H5107.7 (12)
O7Wii—Na1—O5W81.95 (3)H4—O2W—H5104.9 (17)
O4W—Na1—O5W73.77 (3)Na1—O3W—H6115.5 (12)
O2W—Na1—Na2133.97 (3)Na1—O3W—H7114.8 (12)
O8Wi—Na1—Na292.44 (3)H6—O3W—H7107.3 (16)
O3W—Na1—Na290.59 (3)Na2—O4W—Na189.36 (3)
O7Wii—Na1—Na2129.14 (3)Na2—O4W—H8118.0 (12)
O4W—Na1—Na244.70 (2)Na1—O4W—H8104.6 (12)
O5W—Na1—Na247.37 (2)Na2—O4W—H9126.4 (12)
O2W—Na1—Na2i91.59 (3)Na1—O4W—H9114.8 (12)
O8Wi—Na1—Na2i37.66 (2)H8—O4W—H9101.9 (16)
O3W—Na1—Na2i68.95 (3)Na1—O5W—Na285.62 (3)
O7Wii—Na1—Na2i73.33 (2)Na1—O5W—H10106.1 (12)
O4W—Na1—Na2i150.84 (3)Na2—O5W—H1098.3 (12)
O5W—Na1—Na2i123.64 (3)Na1—O5W—H1196.4 (12)
Na2—Na1—Na2i126.910 (14)Na2—O5W—H11151.7 (12)
O2W—Na1—Na2ii67.43 (3)H10—O5W—H11108.1 (17)
O8Wi—Na1—Na2ii74.69 (3)Na2—O6W—Na2iii89.73 (4)
O3W—Na1—Na2ii107.28 (3)Na2—O6W—H12129.9 (12)
O7Wii—Na1—Na2ii29.93 (2)Na2iii—O6W—H1297.0 (12)
O4W—Na1—Na2ii151.96 (3)Na2—O6W—H13122.1 (11)
O5W—Na1—Na2ii110.68 (3)Na2iii—O6W—H13102.4 (12)
Na2—Na1—Na2ii155.42 (2)H12—O6W—H13104.8 (16)
Na2i—Na1—Na2ii50.219 (14)Na2—O7W—Na1v119.02 (4)
O6W—Na2—O7W84.24 (3)Na2—O7W—H14117.8 (12)
O6W—Na2—O4W166.84 (4)Na1v—O7W—H14104.8 (12)
O7W—Na2—O4W83.95 (3)Na2—O7W—H15109.4 (12)
O6W—Na2—O8W98.33 (3)Na1v—O7W—H15101.6 (12)
O7W—Na2—O8W169.19 (4)H14—O7W—H15101.6 (16)
O4W—Na2—O8W94.35 (3)Na1iv—O8W—Na2105.41 (4)
O6W—Na2—O6Wiii90.27 (4)Na1iv—O8W—H16118.7 (12)
O7W—Na2—O6Wiii86.03 (4)Na2—O8W—H16105.2 (12)
O4W—Na2—O6Wiii94.68 (4)Na1iv—O8W—H17115.2 (11)
O8W—Na2—O6Wiii83.46 (3)Na2—O8W—H17105.4 (11)
O6W—Na2—O5W104.04 (4)H16—O8W—H17105.8 (16)
O7W—Na2—O5W108.56 (3)
C6—N1—C2—N32.34 (19)C2—N1—C6—C50.86 (17)
C6—N1—C2—N2178.70 (11)N7—C5—C6—O10.2 (2)
N1—C2—N3—C41.93 (18)C4—C5—C6—O1178.48 (11)
N2—C2—N3—C4178.26 (11)N7—C5—C6—N1179.29 (12)
C2—N3—C4—N9179.45 (11)C4—C5—C6—N10.62 (17)
C2—N3—C4—C50.20 (17)C4—C5—N7—C80.34 (13)
N3—C4—C5—N7179.94 (11)C6—C5—N7—C8178.43 (13)
N9—C4—C5—N70.58 (14)C5—N7—C8—N90.01 (15)
N3—C4—C5—C60.98 (18)N7—C8—N9—C40.35 (15)
N9—C4—C5—C6178.38 (11)N3—C4—N9—C8179.89 (12)
C2—N1—C6—O1179.99 (11)C5—C4—N9—C80.54 (13)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.852 (19)2.115 (19)2.9521 (15)167.2 (16)
O3W—H7···N30.836 (18)1.978 (18)2.7971 (13)166.2 (16)
O4W—H9···N90.802 (19)2.180 (19)2.9814 (14)175.8 (17)
O7W—H15···O3W0.808 (18)1.956 (18)2.7539 (12)169.6 (17)
O6W—H12···O2Wiv0.818 (18)1.979 (19)2.7890 (13)170.3 (17)
O3W—H6···O5Wi0.809 (18)2.132 (18)2.9149 (12)162.9 (16)
O2W—H4···N9ii0.785 (18)2.001 (18)2.7806 (13)172.1 (17)
O4W—H8···N1vi0.813 (18)1.994 (18)2.8034 (13)173.6 (17)
O5W—H10···O1vi0.826 (18)1.938 (18)2.7551 (12)169.9 (16)
O8W—H16···O1vi0.807 (18)2.030 (18)2.8271 (12)169.5 (16)
O5W—H11···O1vii0.814 (18)1.976 (19)2.7770 (13)167.8 (16)
O6W—H13···N7viii0.845 (18)2.072 (18)2.9081 (13)170.2 (16)
O7W—H14···O1viii0.839 (18)1.974 (18)2.7815 (12)161.2 (16)
O8W—H17···N7ix0.836 (18)1.956 (18)2.7853 (14)171.4 (16)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_125K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.584 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5297 (2) ÅCell parameters from 7204 reflections
b = 11.67487 (19) Åθ = 2.6–29.6°
c = 11.1843 (2) ŵ = 0.20 mm1
β = 101.584 (2)°T = 125 K
V = 1346.91 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3774 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3060 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.053
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.845, Tmax = 1.000l = 1514
12905 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: difference Fourier map
wR(F2) = 0.083Only H-atom coordinates refined
S = 1.06 w = 1/[σ2(Fo2) + (0.0353P)2 + 0.6901P]
where P = (Fo2 + 2Fc2)/3
3774 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.53 e Å3
0 restraintsΔρmin = 0.30 e Å3
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*/Ueq
N10.65496 (10)0.48289 (8)0.34803 (9)0.01227 (19)
C20.52573 (11)0.48320 (9)0.33934 (11)0.0130 (2)
N30.45246 (9)0.40244 (8)0.37665 (9)0.0129 (2)
C40.52340 (11)0.31327 (9)0.43252 (10)0.0113 (2)
C50.65768 (11)0.30520 (9)0.44957 (11)0.0114 (2)
C60.72601 (11)0.39387 (9)0.40435 (10)0.0111 (2)
N70.69791 (10)0.20360 (8)0.50939 (9)0.0138 (2)
C80.58572 (11)0.15757 (10)0.52394 (12)0.0148 (2)
H10.5855 (15)0.0871 (14)0.5626 (15)0.018*
N90.47618 (10)0.21795 (8)0.47966 (10)0.0138 (2)
N20.46144 (11)0.57500 (9)0.27884 (11)0.0190 (2)
H20.3825 (17)0.5870 (14)0.2904 (15)0.023*
H30.5114 (17)0.6357 (15)0.2729 (15)0.023*
O10.85034 (8)0.39324 (7)0.41325 (8)0.01242 (16)
Na10.11563 (4)0.25433 (4)0.18360 (4)0.01247 (11)
Na20.04856 (5)0.04509 (4)0.37253 (4)0.01257 (11)
O2W0.30733 (9)0.32581 (7)0.13599 (9)0.01531 (17)
H40.3527 (16)0.3079 (14)0.0903 (16)0.018*
H50.3580 (16)0.3421 (14)0.2030 (16)0.018*
O3W0.18433 (9)0.38028 (7)0.35536 (8)0.01443 (17)
H60.1453 (16)0.4415 (14)0.3520 (15)0.017*
H70.2631 (17)0.3946 (14)0.3736 (15)0.017*
O4W0.24334 (9)0.11491 (7)0.32006 (9)0.01374 (17)
H80.2769 (15)0.0776 (14)0.2742 (15)0.016*
H90.3051 (17)0.1419 (14)0.3657 (15)0.016*
O5W0.00209 (9)0.06873 (7)0.14522 (8)0.01291 (16)
H100.0499 (16)0.0214 (14)0.1250 (14)0.015*
H110.0494 (16)0.0866 (14)0.0806 (16)0.015*
O6W0.15486 (9)0.02106 (7)0.42388 (8)0.01525 (18)
H120.2060 (16)0.0300 (15)0.4075 (15)0.018*
H130.2001 (16)0.0769 (14)0.4407 (15)0.018*
O7W0.04312 (9)0.22701 (7)0.46310 (8)0.01406 (17)
H140.0257 (17)0.2631 (14)0.4486 (15)0.017*
H150.0932 (16)0.2704 (14)0.4370 (15)0.017*
O8W0.08246 (8)0.14990 (7)0.31512 (9)0.01287 (17)
H160.1069 (15)0.1456 (13)0.2536 (16)0.015*
H170.1462 (16)0.1720 (13)0.3664 (15)0.015*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0114 (5)0.0129 (4)0.0125 (5)0.0011 (3)0.0024 (4)0.0017 (3)
C20.0122 (5)0.0137 (5)0.0127 (6)0.0006 (4)0.0017 (4)0.0005 (4)
N30.0101 (5)0.0143 (4)0.0145 (5)0.0009 (3)0.0027 (4)0.0009 (4)
C40.0099 (5)0.0142 (5)0.0097 (5)0.0011 (4)0.0020 (4)0.0008 (4)
C50.0091 (5)0.0127 (5)0.0121 (5)0.0012 (4)0.0018 (4)0.0015 (4)
C60.0105 (5)0.0134 (4)0.0098 (5)0.0006 (4)0.0027 (4)0.0010 (4)
N70.0125 (5)0.0133 (4)0.0151 (5)0.0019 (3)0.0019 (4)0.0034 (4)
C80.0127 (5)0.0151 (5)0.0167 (6)0.0001 (4)0.0032 (4)0.0021 (4)
N90.0107 (5)0.0147 (4)0.0164 (5)0.0001 (3)0.0037 (4)0.0018 (4)
N20.0134 (5)0.0171 (5)0.0264 (6)0.0031 (4)0.0037 (4)0.0079 (4)
O10.0076 (4)0.0162 (4)0.0136 (4)0.0013 (3)0.0024 (3)0.0005 (3)
Na10.0121 (2)0.0119 (2)0.0136 (2)0.00051 (16)0.00294 (18)0.00013 (16)
Na20.0134 (2)0.0116 (2)0.0133 (2)0.00019 (16)0.00430 (18)0.00019 (16)
O2W0.0124 (4)0.0203 (4)0.0141 (5)0.0007 (3)0.0046 (3)0.0023 (3)
O3W0.0099 (4)0.0132 (4)0.0206 (5)0.0004 (3)0.0041 (3)0.0018 (3)
O4W0.0112 (4)0.0150 (4)0.0154 (4)0.0004 (3)0.0036 (3)0.0035 (3)
O5W0.0136 (4)0.0128 (3)0.0117 (4)0.0021 (3)0.0011 (3)0.0005 (3)
O6W0.0125 (4)0.0136 (4)0.0205 (5)0.0009 (3)0.0055 (3)0.0031 (3)
O7W0.0134 (4)0.0129 (3)0.0167 (4)0.0020 (3)0.0049 (3)0.0008 (3)
O8W0.0109 (4)0.0164 (4)0.0114 (4)0.0007 (3)0.0023 (3)0.0020 (3)
Geometric parameters (Å, º) top
N1—C21.3446 (15)Na1—Na2ii4.1351 (7)
N1—C61.3592 (15)Na2—O6W2.3432 (9)
C2—N31.3370 (14)Na2—O7W2.3586 (9)
C2—N21.3714 (15)Na2—O4W2.3871 (9)
N3—C41.3583 (15)Na2—O8W2.4113 (9)
C4—N91.3670 (14)Na2—O6Wiii2.4516 (11)
C4—C51.3914 (15)Na2—O5W2.5059 (10)
C5—N71.3857 (14)Na2—Na2iii3.3847 (9)
C5—C61.4111 (14)O2W—H40.794 (17)
C6—O11.2929 (14)O2W—H50.850 (18)
N7—C81.3372 (15)O3W—H60.821 (17)
C8—N91.3576 (15)O3W—H70.830 (17)
C8—H10.930 (16)O4W—H80.807 (17)
N2—H20.877 (17)O4W—H90.805 (18)
N2—H30.893 (18)O5W—H100.840 (17)
Na1—O2W2.3422 (9)O5W—H110.818 (17)
Na1—O8Wi2.3691 (9)O6W—H120.800 (18)
Na1—O3W2.4120 (10)O6W—H130.851 (17)
Na1—O7Wii2.4404 (10)O7W—H140.825 (17)
Na1—O4W2.4419 (10)O7W—H150.825 (17)
Na1—O5W2.4904 (9)O8W—H160.783 (17)
Na1—Na23.3956 (6)O8W—H170.831 (17)
Na1—Na2i3.8041 (6)
C2—N1—C6119.37 (9)O4W—Na2—O5W74.41 (3)
N3—C2—N1127.92 (10)O8W—Na2—O5W81.17 (3)
N3—C2—N2116.51 (11)O6Wiii—Na2—O5W160.30 (3)
N1—C2—N2115.46 (10)O6W—Na2—Na2iii46.41 (3)
C2—N3—C4112.68 (10)O7W—Na2—Na2iii83.16 (3)
N3—C4—N9126.32 (10)O4W—Na2—Na2iii137.16 (3)
N3—C4—C5124.39 (10)O8W—Na2—Na2iii90.95 (3)
N9—C4—C5109.29 (10)O6Wiii—Na2—Na2iii43.81 (2)
N7—C5—C4109.14 (9)O5W—Na2—Na2iii148.23 (3)
N7—C5—C6132.27 (10)O6W—Na2—Na1123.59 (3)
C4—C5—C6118.58 (10)O7W—Na2—Na169.24 (2)
O1—C6—N1119.65 (10)O4W—Na2—Na145.98 (2)
O1—C6—C5123.33 (10)O8W—Na2—Na1116.94 (3)
N1—C6—C5117.02 (10)O6Wiii—Na2—Na1133.74 (3)
C8—N7—C5102.17 (9)O5W—Na2—Na146.99 (2)
N7—C8—N9116.97 (10)Na2iii—Na2—Na1152.11 (2)
N7—C8—H1119.8 (10)O6W—Na2—Na1iv61.71 (2)
N9—C8—H1123.2 (10)O7W—Na2—Na1iv145.58 (3)
C8—N9—C4102.43 (9)O4W—Na2—Na1iv130.43 (3)
C2—N2—H2116.1 (11)O8W—Na2—Na1iv36.89 (2)
C2—N2—H3114.6 (11)O6Wiii—Na2—Na1iv88.84 (2)
H2—N2—H3118.3 (15)O5W—Na2—Na1iv86.20 (2)
O2W—Na1—O8Wi129.29 (3)Na2iii—Na2—Na1iv69.952 (16)
O2W—Na1—O3W80.18 (3)Na1—Na2—Na1iv133.133 (15)
O8Wi—Na1—O3W80.28 (3)O6W—Na2—Na1v82.63 (3)
O2W—Na1—O7Wii81.23 (3)O7W—Na2—Na1v31.08 (2)
O8Wi—Na1—O7Wii82.35 (3)O4W—Na2—Na1v90.20 (3)
O3W—Na1—O7Wii137.17 (3)O8W—Na2—Na1v138.53 (3)
O2W—Na1—O4W89.31 (3)O6Wiii—Na2—Na1v55.11 (2)
O8Wi—Na1—O4W133.30 (3)O5W—Na2—Na1v139.18 (2)
O3W—Na1—O4W82.48 (3)Na2iii—Na2—Na1v59.791 (15)
O7Wii—Na1—O4W135.43 (3)Na1—Na2—Na1v95.420 (11)
O2W—Na1—O5W133.84 (3)Na1iv—Na2—Na1v129.743 (13)
O8Wi—Na1—O5W90.19 (3)Na1—O2W—H4135.2 (12)
O3W—Na1—O5W136.63 (3)Na1—O2W—H5107.2 (11)
O7Wii—Na1—O5W81.93 (3)H4—O2W—H5105.9 (16)
O4W—Na1—O5W73.76 (3)Na1—O3W—H6115.3 (11)
O2W—Na1—Na2133.96 (3)Na1—O3W—H7116.4 (11)
O8Wi—Na1—Na292.43 (3)H6—O3W—H7107.5 (16)
O3W—Na1—Na290.55 (3)Na2—O4W—Na189.36 (3)
O7Wii—Na1—Na2129.13 (3)Na2—O4W—H8118.6 (11)
O4W—Na1—Na244.66 (2)Na1—O4W—H8102.7 (11)
O5W—Na1—Na247.38 (2)Na2—O4W—H9127.0 (12)
O2W—Na1—Na2i91.63 (3)Na1—O4W—H9114.1 (11)
O8Wi—Na1—Na2i37.66 (2)H8—O4W—H9102.3 (16)
O3W—Na1—Na2i68.97 (2)Na1—O5W—Na285.63 (3)
O7Wii—Na1—Na2i73.38 (2)Na1—O5W—H10106.9 (11)
O4W—Na1—Na2i150.81 (3)Na2—O5W—H10100.6 (11)
O5W—Na1—Na2i123.64 (3)Na1—O5W—H1197.1 (11)
Na2—Na1—Na2i126.887 (13)Na2—O5W—H11153.1 (11)
O2W—Na1—Na2ii67.44 (3)H10—O5W—H11104.1 (15)
O8Wi—Na1—Na2ii74.69 (2)Na2—O6W—Na2iii89.78 (3)
O3W—Na1—Na2ii107.34 (3)Na2—O6W—H12129.8 (12)
O7Wii—Na1—Na2ii29.93 (2)Na2iii—O6W—H1297.9 (12)
O4W—Na1—Na2ii151.99 (3)Na2—O6W—H13122.8 (11)
O5W—Na1—Na2ii110.65 (3)Na2iii—O6W—H13102.0 (11)
Na2—Na1—Na2ii155.40 (2)H12—O6W—H13104.0 (16)
Na2i—Na1—Na2ii50.258 (13)Na2—O7W—Na1v118.99 (4)
O6W—Na2—O7W84.28 (3)Na2—O7W—H14118.1 (11)
O6W—Na2—O4W166.89 (4)Na1v—O7W—H14103.7 (11)
O7W—Na2—O4W83.93 (3)Na2—O7W—H15109.1 (11)
O6W—Na2—O8W98.26 (3)Na1v—O7W—H15102.2 (11)
O7W—Na2—O8W169.15 (4)H14—O7W—H15102.4 (15)
O4W—Na2—O8W94.39 (3)Na1iv—O8W—Na2105.45 (3)
O6W—Na2—O6Wiii90.23 (3)Na1iv—O8W—H16118.8 (12)
O7W—Na2—O6Wiii86.03 (3)Na2—O8W—H16105.4 (12)
O4W—Na2—O6Wiii94.67 (3)Na1iv—O8W—H17116.0 (11)
O8W—Na2—O6Wiii83.43 (3)Na2—O8W—H17104.6 (11)
O6W—Na2—O5W104.06 (4)H16—O8W—H17105.3 (16)
O7W—Na2—O5W108.54 (3)
C6—N1—C2—N32.48 (19)C2—N1—C6—C50.76 (16)
C6—N1—C2—N2178.65 (11)N7—C5—C6—O10.1 (2)
N1—C2—N3—C42.11 (18)C4—C5—C6—O1178.50 (10)
N2—C2—N3—C4178.24 (10)N7—C5—C6—N1179.31 (11)
C2—N3—C4—N9179.64 (11)C4—C5—C6—N10.89 (16)
C2—N3—C4—C50.18 (17)C4—C5—N7—C80.14 (13)
N3—C4—C5—N7179.99 (11)C6—C5—N7—C8178.40 (13)
N9—C4—C5—N70.45 (13)C5—N7—C8—N90.23 (14)
N3—C4—C5—C61.22 (18)N7—C8—N9—C40.49 (14)
N9—C4—C5—C6178.32 (10)N3—C4—N9—C8179.93 (11)
C2—N1—C6—O1179.83 (10)C5—C4—N9—C80.54 (13)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.850 (18)2.117 (18)2.9544 (14)168.4 (15)
O3W—H7···N30.830 (17)1.990 (17)2.7973 (13)164.0 (16)
O4W—H9···N90.805 (18)2.177 (18)2.9811 (14)176.7 (16)
O7W—H15···O3W0.825 (17)1.937 (17)2.7540 (12)170.1 (16)
O6W—H12···O2Wiv0.800 (18)2.000 (18)2.7911 (12)170.1 (16)
O3W—H6···O5Wi0.821 (17)2.121 (17)2.9186 (12)163.6 (15)
O2W—H4···N9ii0.794 (17)1.990 (18)2.7799 (13)173.0 (16)
O4W—H8···N1vi0.807 (17)2.000 (17)2.8044 (13)175.2 (16)
O5W—H10···O1vi0.840 (17)1.925 (17)2.7566 (11)170.1 (15)
O8W—H16···O1vi0.783 (17)2.056 (18)2.8291 (12)169.1 (16)
O5W—H11···O1vii0.818 (17)1.970 (18)2.7791 (13)170.1 (16)
O6W—H13···N7viii0.851 (17)2.065 (17)2.9078 (13)171.0 (15)
O7W—H14···O1viii0.825 (17)1.991 (17)2.7827 (12)160.6 (15)
O8W—H17···N7ix0.831 (17)1.961 (18)2.7876 (14)172.7 (15)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_150K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.581 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5318 (2) ÅCell parameters from 7122 reflections
b = 11.68404 (19) Åθ = 2.7–29.6°
c = 11.1931 (2) ŵ = 0.20 mm1
β = 101.563 (2)°T = 150 K
V = 1349.40 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3781 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3058 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.052
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.815, Tmax = 1.000l = 1514
12926 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: difference Fourier map
wR(F2) = 0.088Only H-atom coordinates refined
S = 1.05 w = 1/[σ2(Fo2) + (0.0401P)2 + 0.6266P]
where P = (Fo2 + 2Fc2)/3
3781 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.54 e Å3
0 restraintsΔρmin = 0.26 e Å3
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*/Ueq
N10.65506 (10)0.48267 (8)0.34799 (9)0.0138 (2)
C20.52588 (12)0.48291 (9)0.33938 (11)0.0144 (2)
N30.45267 (9)0.40209 (8)0.37648 (10)0.0145 (2)
C40.52371 (11)0.31312 (9)0.43255 (11)0.0126 (2)
C50.65781 (11)0.30506 (9)0.44954 (11)0.0129 (2)
C60.72603 (11)0.39372 (9)0.40422 (10)0.0120 (2)
N70.69808 (10)0.20364 (8)0.50918 (10)0.0157 (2)
C80.58599 (12)0.15765 (10)0.52348 (12)0.0171 (2)
H10.5865 (16)0.0878 (14)0.5632 (15)0.021*
N90.47637 (10)0.21785 (8)0.47934 (10)0.0152 (2)
N20.46148 (11)0.57470 (9)0.27904 (12)0.0223 (2)
H20.3812 (18)0.5862 (15)0.2919 (16)0.027*
H30.5108 (17)0.6347 (16)0.2703 (16)0.027*
O10.85047 (8)0.39317 (7)0.41329 (8)0.01376 (17)
Na10.11571 (5)0.25436 (4)0.18342 (4)0.01420 (11)
Na20.04853 (5)0.04506 (4)0.37241 (4)0.01441 (11)
O2W0.30748 (9)0.32579 (8)0.13576 (9)0.01759 (18)
H40.3540 (17)0.3068 (14)0.0910 (16)0.021*
H50.3593 (17)0.3433 (14)0.2022 (17)0.021*
O3W0.18447 (9)0.38018 (7)0.35525 (9)0.01657 (18)
H60.1456 (17)0.4408 (15)0.3536 (15)0.020*
H70.2627 (18)0.3937 (14)0.3735 (15)0.020*
O4W0.24329 (9)0.11480 (7)0.31972 (9)0.01566 (18)
H80.2776 (16)0.0742 (14)0.2746 (15)0.019*
H90.3043 (17)0.1405 (14)0.3648 (16)0.019*
O5W0.00206 (9)0.06867 (7)0.14520 (8)0.01482 (17)
H100.0500 (16)0.0212 (14)0.1255 (15)0.018*
H110.0481 (17)0.0870 (14)0.0836 (16)0.018*
O6W0.15477 (9)0.02108 (8)0.42398 (9)0.01755 (19)
H120.2049 (17)0.0295 (15)0.4078 (15)0.021*
H130.2007 (16)0.0781 (15)0.4401 (15)0.021*
O7W0.04310 (9)0.22697 (7)0.46286 (8)0.01583 (18)
H140.0263 (17)0.2633 (14)0.4496 (15)0.019*
H150.0935 (16)0.2710 (14)0.4381 (15)0.019*
O8W0.08253 (9)0.14993 (7)0.31515 (9)0.01447 (17)
H160.1075 (16)0.1456 (14)0.2505 (16)0.017*
H170.1449 (16)0.1723 (14)0.3672 (16)0.017*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0129 (5)0.0140 (4)0.0147 (5)0.0011 (3)0.0030 (4)0.0020 (3)
C20.0131 (6)0.0152 (5)0.0144 (6)0.0006 (4)0.0018 (4)0.0005 (4)
N30.0104 (5)0.0158 (4)0.0171 (5)0.0005 (3)0.0024 (4)0.0018 (4)
C40.0102 (5)0.0160 (5)0.0118 (5)0.0008 (4)0.0025 (4)0.0003 (4)
C50.0100 (5)0.0143 (5)0.0141 (6)0.0005 (4)0.0017 (4)0.0018 (4)
C60.0112 (5)0.0151 (5)0.0097 (5)0.0003 (4)0.0022 (4)0.0006 (4)
N70.0145 (5)0.0155 (4)0.0169 (5)0.0021 (4)0.0024 (4)0.0040 (4)
C80.0145 (6)0.0165 (5)0.0202 (6)0.0006 (4)0.0033 (5)0.0031 (4)
N90.0122 (5)0.0160 (4)0.0176 (5)0.0002 (3)0.0035 (4)0.0019 (4)
N20.0164 (6)0.0186 (5)0.0318 (7)0.0037 (4)0.0044 (5)0.0096 (4)
O10.0085 (4)0.0183 (4)0.0145 (4)0.0015 (3)0.0023 (3)0.0002 (3)
Na10.0133 (2)0.0136 (2)0.0157 (3)0.00049 (16)0.00299 (18)0.00010 (17)
Na20.0151 (2)0.0132 (2)0.0157 (2)0.00005 (16)0.00501 (19)0.00015 (17)
O2W0.0141 (4)0.0227 (4)0.0169 (5)0.0012 (3)0.0053 (4)0.0027 (3)
O3W0.0106 (4)0.0150 (4)0.0244 (5)0.0007 (3)0.0043 (4)0.0023 (3)
O4W0.0122 (4)0.0167 (4)0.0183 (5)0.0003 (3)0.0036 (3)0.0042 (3)
O5W0.0157 (4)0.0139 (4)0.0142 (4)0.0026 (3)0.0012 (3)0.0005 (3)
O6W0.0147 (4)0.0154 (4)0.0234 (5)0.0010 (3)0.0059 (4)0.0033 (3)
O7W0.0155 (4)0.0140 (4)0.0187 (5)0.0022 (3)0.0053 (3)0.0007 (3)
O8W0.0129 (4)0.0179 (4)0.0125 (4)0.0010 (3)0.0021 (3)0.0021 (3)
Geometric parameters (Å, º) top
N1—C21.3445 (15)Na1—Na2ii4.1382 (7)
N1—C61.3587 (15)Na2—O6W2.3433 (10)
C2—N31.3368 (14)Na2—O7W2.3599 (9)
C2—N21.3721 (16)Na2—O4W2.3884 (10)
N3—C41.3587 (15)Na2—O8W2.4128 (9)
C4—N91.3663 (14)Na2—O6Wiii2.4537 (11)
C4—C51.3899 (15)Na2—O5W2.5069 (10)
C5—N71.3843 (14)Na2—Na2iii3.3885 (9)
C5—C61.4116 (15)O2W—H40.799 (18)
C6—O11.2941 (14)O2W—H50.855 (19)
N7—C81.3356 (15)O3W—H60.817 (17)
C8—N91.3575 (16)O3W—H70.823 (18)
C8—H10.929 (16)O4W—H80.827 (17)
N2—H20.896 (18)O4W—H90.792 (18)
N2—H30.889 (18)O5W—H100.839 (17)
Na1—O2W2.3435 (10)O5W—H110.789 (18)
Na1—O8Wi2.3713 (10)O6W—H120.789 (18)
Na1—O3W2.4138 (10)O6W—H130.864 (18)
Na1—O4W2.4434 (10)O7W—H140.832 (18)
Na1—O7Wii2.4435 (11)O7W—H150.826 (17)
Na1—O5W2.4932 (10)O8W—H160.820 (18)
Na1—Na23.3994 (6)O8W—H170.828 (18)
Na1—Na2i3.8059 (6)
C2—N1—C6119.31 (10)O4W—Na2—O5W74.36 (3)
N3—C2—N1127.92 (11)O8W—Na2—O5W81.20 (3)
N3—C2—N2116.49 (11)O6Wiii—Na2—O5W160.31 (4)
N1—C2—N2115.48 (10)O6W—Na2—Na2iii46.40 (3)
C2—N3—C4112.67 (10)O7W—Na2—Na2iii83.16 (3)
N3—C4—N9126.22 (10)O4W—Na2—Na2iii137.16 (4)
N3—C4—C5124.43 (10)O8W—Na2—Na2iii90.94 (3)
N9—C4—C5109.34 (10)O6Wiii—Na2—Na2iii43.75 (2)
N7—C5—C4109.19 (9)O5W—Na2—Na2iii148.28 (3)
N7—C5—C6132.27 (11)O6W—Na2—Na1123.62 (3)
C4—C5—C6118.52 (10)O7W—Na2—Na169.20 (2)
O1—C6—N1119.64 (10)O4W—Na2—Na145.95 (2)
O1—C6—C5123.27 (10)O8W—Na2—Na1116.97 (3)
N1—C6—C5117.09 (10)O6Wiii—Na2—Na1133.75 (3)
C8—N7—C5102.09 (10)O5W—Na2—Na147.00 (2)
N7—C8—N9117.10 (10)Na2iii—Na2—Na1152.09 (2)
N7—C8—H1119.4 (10)O6W—Na2—Na1iv61.72 (2)
N9—C8—H1123.5 (10)O7W—Na2—Na1iv145.58 (3)
C8—N9—C4102.28 (10)O4W—Na2—Na1iv130.43 (3)
C2—N2—H2115.3 (11)O8W—Na2—Na1iv36.92 (2)
C2—N2—H3115.3 (12)O6Wiii—Na2—Na1iv88.80 (3)
H2—N2—H3119.4 (16)O5W—Na2—Na1iv86.24 (2)
O2W—Na1—O8Wi129.33 (4)Na2iii—Na2—Na1iv69.951 (16)
O2W—Na1—O3W80.21 (4)Na1—Na2—Na1iv133.177 (15)
O8Wi—Na1—O3W80.29 (3)O6W—Na2—Na1v82.59 (3)
O2W—Na1—O4W89.35 (3)O7W—Na2—Na1v31.11 (2)
O8Wi—Na1—O4W133.26 (4)O4W—Na2—Na1v90.23 (3)
O3W—Na1—O4W82.49 (4)O8W—Na2—Na1v138.48 (3)
O2W—Na1—O7Wii81.24 (4)O6Wiii—Na2—Na1v55.09 (2)
O8Wi—Na1—O7Wii82.36 (3)O5W—Na2—Na1v139.19 (3)
O3W—Na1—O7Wii137.21 (3)Na2iii—Na2—Na1v59.766 (15)
O4W—Na1—O7Wii135.39 (4)Na1—Na2—Na1v95.408 (11)
O2W—Na1—O5W133.84 (4)Na1iv—Na2—Na1v129.716 (13)
O8Wi—Na1—O5W90.18 (3)Na1—O2W—H4135.1 (12)
O3W—Na1—O5W136.57 (4)Na1—O2W—H5108.5 (11)
O4W—Na1—O5W73.67 (3)H4—O2W—H5104.3 (17)
O7Wii—Na1—O5W81.96 (3)Na1—O3W—H6116.1 (12)
O2W—Na1—Na2133.96 (3)Na1—O3W—H7116.1 (12)
O8Wi—Na1—Na292.39 (3)H6—O3W—H7108.1 (16)
O3W—Na1—Na290.51 (3)Na2—O4W—Na189.42 (3)
O4W—Na1—Na244.63 (2)Na2—O4W—H8117.2 (11)
O7Wii—Na1—Na2129.12 (3)Na1—O4W—H8104.7 (11)
O5W—Na1—Na247.34 (2)Na2—O4W—H9126.9 (12)
O2W—Na1—Na2i91.65 (3)Na1—O4W—H9114.8 (12)
O8Wi—Na1—Na2i37.67 (2)H8—O4W—H9102.0 (16)
O3W—Na1—Na2i68.97 (3)Na1—O5W—Na285.67 (3)
O4W—Na1—Na2i150.81 (3)Na1—O5W—H10106.9 (11)
O7Wii—Na1—Na2i73.42 (2)Na2—O5W—H10100.2 (11)
O5W—Na1—Na2i123.67 (3)Na1—O5W—H1196.4 (12)
Na2—Na1—Na2i126.852 (13)Na2—O5W—H11152.3 (12)
O2W—Na1—Na2ii67.46 (3)H10—O5W—H11105.6 (16)
O8Wi—Na1—Na2ii74.71 (3)Na2—O6W—Na2iii89.85 (4)
O3W—Na1—Na2ii107.38 (3)Na2—O6W—H12129.5 (12)
O4W—Na1—Na2ii152.02 (3)Na2iii—O6W—H1297.9 (12)
O7Wii—Na1—Na2ii29.93 (2)Na2—O6W—H13122.4 (11)
O5W—Na1—Na2ii110.68 (3)Na2iii—O6W—H13102.7 (11)
Na2—Na1—Na2ii155.38 (2)H12—O6W—H13104.4 (16)
Na2i—Na1—Na2ii50.285 (13)Na2—O7W—Na1v118.96 (4)
O6W—Na2—O7W84.27 (3)Na2—O7W—H14118.6 (11)
O6W—Na2—O4W166.89 (4)Na1v—O7W—H14102.8 (12)
O7W—Na2—O4W83.94 (3)Na2—O7W—H15110.1 (11)
O6W—Na2—O8W98.29 (3)Na1v—O7W—H15101.0 (12)
O7W—Na2—O8W169.13 (4)H14—O7W—H15102.9 (16)
O4W—Na2—O8W94.36 (3)Na1iv—O8W—Na2105.41 (4)
O6W—Na2—O6Wiii90.15 (4)Na1iv—O8W—H16118.3 (11)
O7W—Na2—O6Wiii86.04 (3)Na2—O8W—H16105.5 (11)
O4W—Na2—O6Wiii94.73 (4)Na1iv—O8W—H17114.9 (11)
O8W—Na2—O6Wiii83.40 (3)Na2—O8W—H17104.5 (11)
O6W—Na2—O5W104.14 (4)H16—O8W—H17106.9 (16)
O7W—Na2—O5W108.52 (3)
C6—N1—C2—N32.62 (19)C2—N1—C6—C50.71 (16)
C6—N1—C2—N2178.70 (11)N7—C5—C6—O10.3 (2)
N1—C2—N3—C42.39 (18)C4—C5—C6—O1178.64 (11)
N2—C2—N3—C4178.44 (11)N7—C5—C6—N1179.28 (12)
C2—N3—C4—N9179.56 (11)C4—C5—C6—N10.93 (17)
C2—N3—C4—C50.45 (17)C4—C5—N7—C80.24 (13)
N3—C4—C5—N7179.80 (11)C6—C5—N7—C8178.22 (13)
N9—C4—C5—N70.56 (14)C5—N7—C8—N90.17 (15)
N3—C4—C5—C61.09 (18)N7—C8—N9—C40.50 (15)
N9—C4—C5—C6178.14 (10)N3—C4—N9—C8179.83 (11)
C2—N1—C6—O1179.70 (10)C5—C4—N9—C80.61 (13)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.855 (19)2.115 (19)2.9566 (15)168.0 (16)
O3W—H7···N30.823 (18)1.997 (18)2.7985 (13)164.3 (16)
O4W—H9···N90.792 (18)2.194 (18)2.9848 (14)176.2 (17)
O7W—H15···O3W0.826 (17)1.940 (18)2.7551 (12)169.2 (17)
O6W—H12···O2Wiv0.789 (18)2.013 (19)2.7945 (13)170.6 (17)
O3W—H6···O5Wi0.817 (17)2.127 (18)2.9218 (12)164.3 (16)
O2W—H4···N9ii0.799 (18)1.988 (18)2.7817 (13)172.1 (16)
O4W—H8···N1vi0.827 (17)1.980 (17)2.8034 (13)173.9 (16)
O5W—H10···O1vi0.839 (17)1.926 (18)2.7570 (11)170.4 (16)
O8W—H16···O1vi0.820 (18)2.021 (18)2.8307 (12)169.1 (16)
O5W—H11···O1vii0.789 (18)2.003 (18)2.7808 (13)168.6 (17)
O6W—H13···N7viii0.864 (18)2.053 (18)2.9075 (13)170.0 (16)
O7W—H14···O1viii0.832 (18)1.985 (18)2.7827 (12)160.3 (16)
O8W—H17···N7ix0.828 (18)1.966 (18)2.7888 (14)172.0 (16)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_175K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.577 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5340 (2) ÅCell parameters from 7028 reflections
b = 11.69648 (19) Åθ = 2.6–29.6°
c = 11.2042 (2) ŵ = 0.20 mm1
β = 101.545 (2)°T = 175 K
V = 1352.54 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3797 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3045 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.051
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.977, Tmax = 1.000l = 1514
12962 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: difference Fourier map
wR(F2) = 0.091Only H-atom coordinates refined
S = 1.08 w = 1/[σ2(Fo2) + (0.0375P)2 + 0.7155P]
where P = (Fo2 + 2Fc2)/3
3797 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.47 e Å3
0 restraintsΔρmin = 0.23 e Å3
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*/Ueq
N10.65512 (10)0.48244 (9)0.34798 (10)0.0156 (2)
C20.52606 (12)0.48245 (10)0.33949 (12)0.0165 (2)
N30.45286 (10)0.40186 (9)0.37636 (10)0.0167 (2)
C40.52390 (12)0.31286 (10)0.43233 (11)0.0142 (2)
C50.65769 (12)0.30512 (10)0.44904 (12)0.0146 (2)
C60.72622 (12)0.39355 (10)0.40418 (11)0.0137 (2)
N70.69824 (11)0.20365 (9)0.50882 (11)0.0183 (2)
C80.58620 (13)0.15774 (11)0.52339 (13)0.0190 (3)
H10.5873 (16)0.0875 (15)0.5627 (16)0.023*
N90.47673 (11)0.21767 (9)0.47920 (11)0.0177 (2)
N20.46152 (13)0.57440 (11)0.27944 (13)0.0254 (3)
H20.3807 (19)0.5855 (16)0.2875 (17)0.030*
H30.5107 (19)0.6349 (17)0.2722 (17)0.030*
O10.85044 (8)0.39312 (7)0.41319 (8)0.01606 (19)
Na10.11585 (5)0.25441 (4)0.18321 (5)0.01652 (12)
Na20.04851 (5)0.04510 (4)0.37224 (5)0.01659 (12)
O2W0.30757 (10)0.32572 (9)0.13555 (10)0.0205 (2)
H40.3521 (18)0.3073 (15)0.0920 (18)0.025*
H50.3594 (18)0.3419 (15)0.2049 (18)0.025*
O3W0.18468 (10)0.38008 (8)0.35509 (9)0.0192 (2)
H60.1476 (18)0.4406 (16)0.3523 (16)0.023*
H70.2641 (19)0.3931 (15)0.3722 (16)0.023*
O4W0.24331 (10)0.11476 (8)0.31955 (10)0.01802 (19)
H80.2787 (17)0.0762 (15)0.2747 (16)0.022*
H90.3044 (18)0.1404 (15)0.3647 (17)0.022*
O5W0.00206 (10)0.06869 (8)0.14499 (9)0.01695 (18)
H100.0502 (17)0.0226 (15)0.1253 (16)0.020*
H110.0497 (18)0.0869 (15)0.0812 (17)0.020*
O6W0.15495 (10)0.02091 (8)0.42385 (9)0.0204 (2)
H120.2070 (18)0.0317 (16)0.4087 (16)0.024*
H130.1997 (18)0.0763 (16)0.4413 (17)0.024*
O7W0.04302 (10)0.22693 (8)0.46267 (9)0.01840 (19)
H140.0258 (19)0.2632 (15)0.4468 (16)0.022*
H150.0919 (18)0.2699 (15)0.4377 (17)0.022*
O8W0.08245 (9)0.14993 (8)0.31525 (9)0.01689 (19)
H160.1095 (17)0.1451 (15)0.2533 (17)0.020*
H170.1471 (18)0.1725 (15)0.3664 (17)0.020*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0138 (5)0.0169 (4)0.0161 (5)0.0016 (4)0.0032 (4)0.0019 (4)
C20.0151 (6)0.0171 (5)0.0170 (6)0.0011 (4)0.0029 (5)0.0012 (4)
N30.0111 (5)0.0193 (5)0.0195 (6)0.0009 (4)0.0027 (4)0.0016 (4)
C40.0115 (6)0.0181 (5)0.0132 (6)0.0008 (4)0.0027 (4)0.0002 (4)
C50.0113 (6)0.0168 (5)0.0160 (6)0.0006 (4)0.0033 (4)0.0016 (4)
C60.0116 (6)0.0171 (5)0.0127 (6)0.0010 (4)0.0032 (4)0.0015 (4)
N70.0150 (5)0.0183 (5)0.0212 (6)0.0024 (4)0.0027 (4)0.0044 (4)
C80.0171 (6)0.0193 (6)0.0204 (7)0.0002 (5)0.0036 (5)0.0047 (5)
N90.0130 (5)0.0194 (5)0.0208 (6)0.0004 (4)0.0042 (4)0.0034 (4)
N20.0175 (6)0.0222 (5)0.0364 (7)0.0043 (4)0.0049 (5)0.0108 (5)
O10.0092 (4)0.0212 (4)0.0181 (5)0.0014 (3)0.0035 (3)0.0003 (3)
Na10.0151 (3)0.0165 (2)0.0180 (3)0.00069 (18)0.0036 (2)0.00009 (19)
Na20.0171 (3)0.0159 (2)0.0177 (3)0.00010 (18)0.0057 (2)0.00003 (18)
O2W0.0162 (5)0.0273 (5)0.0192 (5)0.0013 (4)0.0068 (4)0.0033 (4)
O3W0.0125 (5)0.0184 (4)0.0274 (6)0.0007 (3)0.0056 (4)0.0022 (4)
O4W0.0144 (5)0.0207 (4)0.0195 (5)0.0003 (3)0.0048 (4)0.0042 (4)
O5W0.0171 (5)0.0174 (4)0.0157 (5)0.0031 (3)0.0018 (4)0.0009 (3)
O6W0.0166 (5)0.0189 (4)0.0269 (5)0.0009 (4)0.0076 (4)0.0036 (4)
O7W0.0175 (5)0.0169 (4)0.0218 (5)0.0029 (3)0.0063 (4)0.0017 (3)
O8W0.0141 (4)0.0212 (4)0.0154 (5)0.0009 (3)0.0030 (4)0.0027 (3)
Geometric parameters (Å, º) top
N1—C21.3437 (16)Na1—Na2ii4.1415 (7)
N1—C61.3600 (16)Na2—O6W2.3460 (11)
C2—N31.3347 (15)Na2—O7W2.3614 (10)
C2—N21.3742 (17)Na2—O4W2.3892 (10)
N3—C41.3597 (16)Na2—O8W2.4148 (10)
C4—N91.3663 (15)Na2—O6Wiii2.4592 (12)
C4—C51.3870 (17)Na2—O5W2.5100 (11)
C5—N71.3874 (16)Na2—Na2iii3.3947 (10)
C5—C61.4103 (16)O2W—H40.77 (2)
C6—O11.2921 (15)O2W—H50.88 (2)
N7—C81.3360 (16)O3W—H60.806 (19)
C8—N91.3557 (17)O3W—H70.835 (19)
C8—H10.931 (17)O4W—H80.818 (19)
N2—H20.88 (2)O4W—H90.794 (19)
N2—H30.89 (2)O5W—H100.831 (18)
Na1—O2W2.3433 (11)O5W—H110.815 (19)
Na1—O8Wi2.3728 (10)O6W—H120.82 (2)
Na1—O3W2.4158 (11)O6W—H130.847 (19)
Na1—O4W2.4460 (11)O7W—H140.828 (19)
Na1—O7Wii2.4461 (12)O7W—H150.809 (19)
Na1—O5W2.4964 (10)O8W—H160.804 (19)
Na1—Na23.4035 (7)O8W—H170.840 (19)
Na1—Na2i3.8097 (7)
C2—N1—C6119.24 (10)O4W—Na2—O5W74.35 (4)
N3—C2—N1128.10 (12)O8W—Na2—O5W81.27 (4)
N3—C2—N2116.38 (12)O6Wiii—Na2—O5W160.33 (4)
N1—C2—N2115.42 (11)O6W—Na2—Na2iii46.42 (3)
C2—N3—C4112.63 (10)O7W—Na2—Na2iii83.15 (3)
N3—C4—N9126.31 (11)O4W—Na2—Na2iii137.12 (4)
N3—C4—C5124.25 (11)O8W—Na2—Na2iii90.85 (3)
N9—C4—C5109.44 (11)O6Wiii—Na2—Na2iii43.71 (3)
C4—C5—N7109.11 (10)O5W—Na2—Na2iii148.32 (4)
C4—C5—C6118.87 (11)O6W—Na2—Na1123.68 (3)
N7—C5—C6132.01 (11)O7W—Na2—Na169.22 (3)
O1—C6—N1119.63 (11)O4W—Na2—Na145.94 (3)
O1—C6—C5123.50 (11)O8W—Na2—Na1117.04 (3)
N1—C6—C5116.87 (11)O6Wiii—Na2—Na1133.70 (3)
C8—N7—C5102.04 (10)O5W—Na2—Na147.00 (2)
N7—C8—N9117.08 (11)Na2iii—Na2—Na1152.10 (3)
N7—C8—H1119.0 (11)O6W—Na2—Na1iv61.63 (3)
N9—C8—H1123.9 (11)O7W—Na2—Na1iv145.53 (3)
C8—N9—C4102.33 (10)O4W—Na2—Na1iv130.45 (3)
C2—N2—H2117.2 (12)O8W—Na2—Na1iv36.89 (2)
C2—N2—H3115.2 (13)O6Wiii—Na2—Na1iv88.80 (3)
H2—N2—H3118.9 (17)O5W—Na2—Na1iv86.30 (3)
O2W—Na1—O8Wi129.34 (4)Na2iii—Na2—Na1iv69.907 (17)
O2W—Na1—O3W80.23 (4)Na1—Na2—Na1iv133.235 (16)
O8Wi—Na1—O3W80.30 (4)O6W—Na2—Na1v82.65 (3)
O2W—Na1—O4W89.40 (4)O7W—Na2—Na1v31.12 (3)
O8Wi—Na1—O4W133.19 (4)O4W—Na2—Na1v90.22 (3)
O3W—Na1—O4W82.46 (4)O8W—Na2—Na1v138.41 (3)
O2W—Na1—O7Wii81.28 (4)O6Wiii—Na2—Na1v55.02 (3)
O8Wi—Na1—O7Wii82.34 (4)O5W—Na2—Na1v139.20 (3)
O3W—Na1—O7Wii137.26 (4)Na2iii—Na2—Na1v59.757 (16)
O4W—Na1—O7Wii135.43 (4)Na1—Na2—Na1v95.411 (12)
O2W—Na1—O5W133.83 (4)Na1iv—Na2—Na1v129.664 (14)
O8Wi—Na1—O5W90.17 (4)Na1—O2W—H4134.8 (13)
O3W—Na1—O5W136.54 (4)Na1—O2W—H5106.7 (12)
O4W—Na1—O5W73.63 (4)H4—O2W—H5105.8 (18)
O7Wii—Na1—O5W81.93 (4)Na1—O3W—H6116.0 (13)
O2W—Na1—Na2133.97 (3)Na1—O3W—H7114.9 (12)
O8Wi—Na1—Na292.36 (3)H6—O3W—H7107.8 (17)
O3W—Na1—Na290.48 (3)Na2—O4W—Na189.47 (4)
O4W—Na1—Na244.59 (2)Na2—O4W—H8118.9 (12)
O7Wii—Na1—Na2129.09 (3)Na1—O4W—H8104.2 (12)
O5W—Na1—Na247.34 (3)Na2—O4W—H9126.7 (13)
O2W—Na1—Na2i91.69 (3)Na1—O4W—H9114.8 (13)
O8Wi—Na1—Na2i37.66 (2)H8—O4W—H9100.9 (17)
O3W—Na1—Na2i68.96 (3)Na1—O5W—Na285.66 (3)
O4W—Na1—Na2i150.76 (3)Na1—O5W—H10106.1 (12)
O7Wii—Na1—Na2i73.45 (3)Na2—O5W—H10100.4 (12)
O5W—Na1—Na2i123.67 (3)Na1—O5W—H1197.0 (12)
Na2—Na1—Na2i126.794 (15)Na2—O5W—H11152.4 (12)
O2W—Na1—Na2ii67.48 (3)H10—O5W—H11105.1 (17)
O8Wi—Na1—Na2ii74.71 (3)Na2—O6W—Na2iii89.86 (4)
O3W—Na1—Na2ii107.44 (3)Na2—O6W—H12130.2 (13)
O4W—Na1—Na2ii152.09 (3)Na2iii—O6W—H1296.8 (13)
O7Wii—Na1—Na2ii29.93 (2)Na2—O6W—H13122.9 (12)
O5W—Na1—Na2ii110.66 (3)Na2iii—O6W—H13101.3 (12)
Na2—Na1—Na2ii155.35 (2)H12—O6W—H13104.1 (17)
Na2i—Na1—Na2ii50.336 (14)Na2—O7W—Na1v118.95 (4)
O6W—Na2—O7W84.31 (4)Na2—O7W—H14117.7 (12)
O6W—Na2—O4W166.96 (4)Na1v—O7W—H14104.8 (12)
O7W—Na2—O4W83.97 (4)Na2—O7W—H15109.8 (13)
O6W—Na2—O8W98.17 (4)Na1v—O7W—H15101.6 (13)
O7W—Na2—O8W169.09 (4)H14—O7W—H15101.4 (17)
O4W—Na2—O8W94.41 (4)Na1iv—O8W—Na2105.45 (4)
O6W—Na2—O6Wiii90.13 (4)Na1iv—O8W—H16120.3 (12)
O7W—Na2—O6Wiii85.98 (4)Na2—O8W—H16105.0 (12)
O4W—Na2—O6Wiii94.72 (4)Na1iv—O8W—H17116.2 (12)
O8W—Na2—O6Wiii83.39 (4)Na2—O8W—H17105.1 (12)
O6W—Na2—O5W104.14 (4)H16—O8W—H17103.4 (17)
O7W—Na2—O5W108.53 (4)
C6—N1—C2—N32.7 (2)C2—N1—C6—C50.84 (18)
C6—N1—C2—N2178.87 (12)C4—C5—C6—O1178.65 (11)
N1—C2—N3—C42.4 (2)N7—C5—C6—O10.1 (2)
N2—C2—N3—C4178.57 (12)C4—C5—C6—N10.79 (18)
C2—N3—C4—N9179.68 (12)N7—C5—C6—N1179.37 (13)
C2—N3—C4—C50.47 (18)C4—C5—N7—C80.15 (14)
N3—C4—C5—N7179.88 (12)C6—C5—N7—C8178.54 (14)
N9—C4—C5—N70.56 (15)C5—N7—C8—N90.33 (16)
N3—C4—C5—C60.99 (19)N7—C8—N9—C40.66 (16)
N9—C4—C5—C6178.33 (11)N3—C4—N9—C8179.99 (13)
C2—N1—C6—O1179.70 (11)C5—C4—N9—C80.70 (14)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.88 (2)2.10 (2)2.9601 (16)168.5 (17)
O3W—H7···N30.835 (19)1.982 (19)2.7988 (14)165.9 (17)
O4W—H9···N90.794 (19)2.20 (2)2.9889 (15)176.1 (18)
O7W—H15···O3W0.809 (19)1.958 (19)2.7583 (13)170.2 (18)
O6W—H12···O2Wiv0.82 (2)1.98 (2)2.7949 (14)170.0 (18)
O3W—H6···O5Wi0.806 (19)2.148 (19)2.9268 (13)162.5 (17)
O2W—H4···N9ii0.77 (2)2.02 (2)2.7841 (14)171.9 (18)
O4W—H8···N1vi0.818 (19)1.991 (19)2.8049 (14)173.2 (17)
O5W—H10···O1vi0.831 (18)1.938 (19)2.7587 (12)169.1 (17)
O8W—H16···O1vi0.804 (19)2.042 (19)2.8335 (13)168.0 (17)
O5W—H11···O1vii0.815 (19)1.98 (2)2.7828 (14)169.2 (17)
O6W—H13···N7viii0.847 (19)2.067 (19)2.9079 (14)172.0 (17)
O7W—H14···O1viii0.828 (19)1.989 (19)2.7840 (13)160.9 (17)
O8W—H17···N7ix0.840 (19)1.957 (19)2.7919 (15)172.3 (17)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_200K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.573 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5373 (2) ÅCell parameters from 6918 reflections
b = 11.70992 (19) Åθ = 2.5–29.6°
c = 11.2176 (2) ŵ = 0.19 mm1
β = 101.523 (2)°T = 200 K
V = 1356.25 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3812 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3033 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.048
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.963, Tmax = 1.000l = 1514
13069 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: difference Fourier map
wR(F2) = 0.095Only H-atom coordinates refined
S = 1.11 w = 1/[σ2(Fo2) + (0.042P)2 + 0.533P]
where P = (Fo2 + 2Fc2)/3
3812 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 0.24 e Å3
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*/Ueq
N10.65528 (10)0.48205 (9)0.34800 (10)0.0176 (2)
C20.52631 (12)0.48216 (10)0.33982 (12)0.0183 (2)
N30.45291 (10)0.40141 (9)0.37618 (10)0.0185 (2)
C40.52400 (11)0.31266 (10)0.43197 (11)0.0158 (2)
C50.65793 (11)0.30494 (10)0.44881 (12)0.0161 (2)
C60.72631 (12)0.39342 (10)0.40418 (11)0.0154 (2)
N70.69847 (11)0.20366 (9)0.50855 (11)0.0203 (2)
C80.58652 (13)0.15778 (11)0.52314 (13)0.0213 (3)
H10.5868 (16)0.0872 (15)0.5624 (16)0.026*
N90.47698 (10)0.21762 (9)0.47889 (11)0.0198 (2)
N20.46164 (13)0.57397 (11)0.27988 (13)0.0289 (3)
H20.380 (2)0.5847 (17)0.2893 (17)0.035*
H30.5086 (19)0.6331 (17)0.2695 (17)0.035*
O10.85050 (8)0.39295 (7)0.41300 (8)0.01814 (19)
Na10.11604 (5)0.25451 (4)0.18305 (5)0.01856 (12)
Na20.04853 (5)0.04511 (4)0.37209 (5)0.01874 (12)
O2W0.30795 (10)0.32576 (9)0.13538 (10)0.0230 (2)
H40.3515 (18)0.3065 (15)0.0909 (18)0.028*
H50.3607 (18)0.3415 (15)0.2057 (18)0.028*
O3W0.18495 (10)0.38009 (8)0.35512 (9)0.0216 (2)
H60.1473 (18)0.4417 (16)0.3530 (16)0.026*
H70.2626 (19)0.3938 (15)0.3732 (16)0.026*
O4W0.24354 (9)0.11472 (8)0.31941 (10)0.0202 (2)
H80.2775 (17)0.0759 (15)0.2730 (16)0.024*
H90.3038 (18)0.1404 (15)0.3650 (17)0.024*
O5W0.00179 (10)0.06878 (8)0.14510 (9)0.01921 (19)
H100.0483 (17)0.0214 (16)0.1244 (16)0.023*
H110.0475 (18)0.0864 (15)0.0836 (17)0.023*
O6W0.15479 (10)0.02084 (8)0.42396 (10)0.0230 (2)
H120.2061 (18)0.0310 (17)0.4077 (16)0.028*
H130.2002 (18)0.0763 (16)0.4406 (16)0.028*
O7W0.04301 (10)0.22688 (8)0.46230 (9)0.0207 (2)
H140.0260 (19)0.2638 (15)0.4475 (16)0.025*
H150.0928 (18)0.2695 (16)0.4382 (16)0.025*
O8W0.08241 (9)0.14989 (8)0.31531 (9)0.01874 (19)
H160.1088 (17)0.1468 (14)0.2517 (17)0.022*
H170.1451 (17)0.1720 (15)0.3654 (17)0.022*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0154 (5)0.0184 (4)0.0192 (5)0.0016 (4)0.0037 (4)0.0023 (4)
C20.0157 (6)0.0195 (5)0.0195 (6)0.0011 (4)0.0030 (5)0.0020 (4)
N30.0127 (5)0.0204 (5)0.0222 (6)0.0008 (4)0.0029 (4)0.0021 (4)
C40.0124 (5)0.0192 (5)0.0159 (6)0.0011 (4)0.0030 (4)0.0002 (4)
C50.0122 (5)0.0180 (5)0.0182 (6)0.0007 (4)0.0030 (4)0.0018 (4)
C60.0127 (6)0.0186 (5)0.0151 (6)0.0011 (4)0.0031 (4)0.0012 (4)
N70.0166 (5)0.0198 (5)0.0242 (6)0.0025 (4)0.0029 (4)0.0057 (4)
C80.0181 (6)0.0210 (6)0.0249 (7)0.0002 (5)0.0041 (5)0.0048 (5)
N90.0147 (5)0.0211 (5)0.0241 (6)0.0011 (4)0.0051 (4)0.0033 (4)
N20.0204 (6)0.0242 (5)0.0420 (8)0.0046 (5)0.0061 (5)0.0123 (5)
O10.0105 (4)0.0231 (4)0.0211 (5)0.0017 (3)0.0040 (3)0.0005 (3)
Na10.0171 (3)0.0184 (2)0.0203 (3)0.00091 (18)0.0039 (2)0.00019 (19)
Na20.0194 (3)0.0178 (2)0.0202 (3)0.00001 (18)0.0066 (2)0.00007 (19)
O2W0.0180 (5)0.0305 (5)0.0219 (5)0.0011 (4)0.0074 (4)0.0034 (4)
O3W0.0143 (5)0.0203 (4)0.0307 (6)0.0006 (3)0.0058 (4)0.0023 (4)
O4W0.0157 (5)0.0225 (4)0.0228 (5)0.0002 (3)0.0049 (4)0.0048 (4)
O5W0.0203 (5)0.0190 (4)0.0175 (5)0.0038 (3)0.0019 (4)0.0016 (3)
O6W0.0188 (5)0.0207 (4)0.0307 (6)0.0008 (4)0.0079 (4)0.0040 (4)
O7W0.0202 (5)0.0187 (4)0.0240 (5)0.0029 (3)0.0067 (4)0.0007 (3)
O8W0.0154 (4)0.0236 (4)0.0169 (5)0.0011 (3)0.0025 (4)0.0021 (3)
Geometric parameters (Å, º) top
N1—C21.3436 (16)Na1—Na2ii4.1458 (7)
N1—C61.3587 (16)Na2—O6W2.3467 (11)
C2—N31.3359 (15)Na2—O7W2.3625 (10)
C2—N21.3745 (17)Na2—O4W2.3919 (10)
N3—C41.3585 (16)Na2—O8W2.4162 (10)
C4—N91.3657 (15)Na2—O6Wiii2.4618 (12)
C4—C51.3889 (16)Na2—O5W2.5104 (11)
C5—N71.3870 (15)Na2—Na2iii3.4014 (10)
C5—C61.4097 (15)O2W—H40.776 (19)
C6—O11.2925 (15)O2W—H50.89 (2)
N7—C81.3358 (16)O3W—H60.821 (19)
C8—N91.3567 (17)O3W—H70.819 (19)
C8—H10.936 (18)O4W—H80.825 (18)
N2—H20.89 (2)O4W—H90.791 (19)
N2—H30.87 (2)O5W—H100.830 (19)
Na1—O2W2.3459 (10)O5W—H110.786 (19)
Na1—O8Wi2.3753 (10)O6W—H120.81 (2)
Na1—O3W2.4199 (11)O6W—H130.849 (19)
Na1—O4W2.4501 (11)O7W—H140.833 (19)
Na1—O7Wii2.4515 (11)O7W—H150.809 (19)
Na1—O5W2.4984 (10)O8W—H160.816 (19)
Na1—Na23.4086 (7)O8W—H170.819 (19)
Na1—Na2i3.8133 (7)
C2—N1—C6119.23 (10)O4W—Na2—O5W74.31 (4)
N3—C2—N1128.16 (11)O8W—Na2—O5W81.33 (4)
N3—C2—N2116.25 (12)O6Wiii—Na2—O5W160.37 (4)
N1—C2—N2115.47 (11)O6W—Na2—Na2iii46.37 (3)
C2—N3—C4112.49 (10)O7W—Na2—Na2iii83.18 (3)
N3—C4—N9126.29 (11)O4W—Na2—Na2iii137.07 (4)
N3—C4—C5124.35 (11)O8W—Na2—Na2iii90.80 (3)
N9—C4—C5109.36 (11)O6Wiii—Na2—Na2iii43.62 (3)
N7—C5—C4109.14 (10)O5W—Na2—Na2iii148.41 (4)
N7—C5—C6132.07 (11)O6W—Na2—Na1123.76 (3)
C4—C5—C6118.78 (11)O7W—Na2—Na169.17 (3)
O1—C6—N1119.62 (10)O4W—Na2—Na145.95 (3)
O1—C6—C5123.44 (11)O8W—Na2—Na1117.11 (3)
N1—C6—C5116.93 (11)O6Wiii—Na2—Na1133.72 (3)
C8—N7—C5102.06 (10)O5W—Na2—Na146.97 (2)
N7—C8—N9117.06 (11)Na2iii—Na2—Na1152.08 (2)
N7—C8—H1119.5 (10)O6W—Na2—Na1iv61.58 (3)
N9—C8—H1123.4 (11)O7W—Na2—Na1iv145.51 (3)
C8—N9—C4102.37 (10)O4W—Na2—Na1iv130.49 (3)
C2—N2—H2116.5 (13)O8W—Na2—Na1iv36.89 (2)
C2—N2—H3116.5 (13)O6Wiii—Na2—Na1iv88.76 (3)
H2—N2—H3119.1 (18)O5W—Na2—Na1iv86.38 (3)
O2W—Na1—O8Wi129.38 (4)Na2iii—Na2—Na1iv69.881 (17)
O2W—Na1—O3W80.26 (4)Na1—Na2—Na1iv133.292 (16)
O8Wi—Na1—O3W80.31 (4)O6W—Na2—Na1v82.63 (3)
O2W—Na1—O4W89.42 (4)O7W—Na2—Na1v31.18 (3)
O8Wi—Na1—O4W133.14 (4)O4W—Na2—Na1v90.20 (3)
O3W—Na1—O4W82.43 (4)O8W—Na2—Na1v138.34 (3)
O2W—Na1—O7Wii81.32 (4)O6Wiii—Na2—Na1v54.97 (3)
O8Wi—Na1—O7Wii82.34 (4)O5W—Na2—Na1v139.19 (3)
O3W—Na1—O7Wii137.33 (4)Na2iii—Na2—Na1v59.732 (16)
O4W—Na1—O7Wii135.43 (4)Na1—Na2—Na1v95.408 (12)
O2W—Na1—O5W133.83 (4)Na1iv—Na2—Na1v129.612 (14)
O8Wi—Na1—O5W90.19 (4)Na1—O2W—H4133.7 (13)
O3W—Na1—O5W136.44 (4)Na1—O2W—H5106.7 (12)
O4W—Na1—O5W73.54 (4)H4—O2W—H5106.6 (18)
O7Wii—Na1—O5W81.97 (4)Na1—O3W—H6116.4 (13)
O2W—Na1—Na2133.97 (3)Na1—O3W—H7116.3 (13)
O8Wi—Na1—Na292.33 (3)H6—O3W—H7106.8 (17)
O3W—Na1—Na290.43 (3)Na2—O4W—Na189.48 (4)
O4W—Na1—Na244.56 (2)Na2—O4W—H8118.1 (12)
O7Wii—Na1—Na2129.05 (3)Na1—O4W—H8103.1 (12)
O5W—Na1—Na247.26 (3)Na2—O4W—H9126.0 (13)
O2W—Na1—Na2i91.74 (3)Na1—O4W—H9114.7 (13)
O8Wi—Na1—Na2i37.64 (2)H8—O4W—H9103.0 (17)
O3W—Na1—Na2i68.98 (3)Na1—O5W—Na285.77 (3)
O4W—Na1—Na2i150.73 (3)Na1—O5W—H10107.9 (12)
O7Wii—Na1—Na2i73.50 (3)Na2—O5W—H10101.1 (12)
O5W—Na1—Na2i123.70 (3)Na1—O5W—H1196.8 (13)
Na2—Na1—Na2i126.741 (14)Na2—O5W—H11152.5 (13)
O2W—Na1—Na2ii67.53 (3)H10—O5W—H11104.0 (18)
O8Wi—Na1—Na2ii74.72 (3)Na2—O6W—Na2iii90.01 (4)
O3W—Na1—Na2ii107.51 (3)Na2—O6W—H12129.6 (13)
O4W—Na1—Na2ii152.12 (3)Na2iii—O6W—H1297.7 (13)
O7Wii—Na1—Na2ii29.93 (2)Na2—O6W—H13123.0 (12)
O5W—Na1—Na2ii110.70 (3)Na2iii—O6W—H13102.0 (12)
Na2—Na1—Na2ii155.30 (2)H12—O6W—H13104.0 (17)
Na2i—Na1—Na2ii50.387 (14)Na2—O7W—Na1v118.89 (4)
O6W—Na2—O7W84.32 (4)Na2—O7W—H14118.5 (12)
O6W—Na2—O4W167.01 (4)Na1v—O7W—H14103.9 (12)
O7W—Na2—O4W83.95 (4)Na2—O7W—H15109.9 (13)
O6W—Na2—O8W98.12 (4)Na1v—O7W—H15100.9 (13)
O7W—Na2—O8W169.09 (4)H14—O7W—H15102.2 (17)
O4W—Na2—O8W94.44 (4)Na1iv—O8W—Na2105.47 (4)
O6W—Na2—O6Wiii89.99 (4)Na1iv—O8W—H16118.8 (12)
O7W—Na2—O6Wiii85.99 (4)Na2—O8W—H16106.4 (12)
O4W—Na2—O6Wiii94.75 (4)Na1iv—O8W—H17115.9 (12)
O8W—Na2—O6Wiii83.38 (4)Na2—O8W—H17105.0 (12)
O6W—Na2—O5W104.27 (4)H16—O8W—H17104.2 (17)
O7W—Na2—O5W108.46 (4)
C6—N1—C2—N33.3 (2)C2—N1—C6—C51.20 (18)
C6—N1—C2—N2178.97 (12)N7—C5—C6—O10.3 (2)
N1—C2—N3—C42.9 (2)C4—C5—C6—O1178.46 (11)
N2—C2—N3—C4178.54 (12)N7—C5—C6—N1179.38 (13)
C2—N3—C4—N9179.99 (12)C4—C5—C6—N10.67 (18)
C2—N3—C4—C50.66 (18)C4—C5—N7—C80.10 (14)
N3—C4—C5—N7179.95 (12)C6—C5—N7—C8178.71 (14)
N9—C4—C5—N70.50 (15)C5—N7—C8—N90.36 (16)
N3—C4—C5—C60.96 (19)N7—C8—N9—C40.65 (16)
N9—C4—C5—C6178.49 (11)N3—C4—N9—C8179.91 (12)
C2—N1—C6—O1179.64 (11)C5—C4—N9—C80.66 (14)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.89 (2)2.09 (2)2.9608 (16)167.8 (17)
O3W—H7···N30.819 (19)2.001 (19)2.7972 (14)164.1 (18)
O4W—H9···N90.791 (19)2.20 (2)2.9908 (15)175.3 (18)
O7W—H15···O3W0.809 (19)1.962 (19)2.7604 (13)169.0 (18)
O6W—H12···O2Wiv0.81 (2)2.00 (2)2.7995 (14)170.7 (18)
O3W—H6···O5Wi0.821 (19)2.140 (19)2.9334 (13)162.5 (17)
O2W—H4···N9ii0.776 (19)2.02 (2)2.7859 (14)170.6 (18)
O4W—H8···N1vi0.825 (18)1.983 (19)2.8067 (14)175.2 (17)
O5W—H10···O1vi0.830 (19)1.938 (19)2.7606 (12)170.9 (17)
O8W—H16···O1vi0.816 (19)2.033 (19)2.8345 (13)167.1 (17)
O5W—H11···O1vii0.786 (19)2.01 (2)2.7899 (14)169.4 (18)
O6W—H13···N7viii0.849 (19)2.067 (19)2.9087 (14)171.2 (17)
O7W—H14···O1viii0.833 (19)1.982 (19)2.7847 (13)161.3 (17)
O8W—H17···N7ix0.819 (19)1.980 (19)2.7944 (15)172.4 (17)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_225K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.569 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5404 (2) ÅCell parameters from 5822 reflections
b = 11.7241 (2) Åθ = 2.6–29.6°
c = 11.2296 (3) ŵ = 0.19 mm1
β = 101.504 (2)°T = 225 K
V = 1359.83 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3824 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3020 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.045
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.780, Tmax = 1.000l = 1514
12552 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: difference Fourier map
wR(F2) = 0.092Only H-atom coordinates refined
S = 1.07 w = 1/[σ2(Fo2) + (0.0411P)2 + 0.5137P]
where P = (Fo2 + 2Fc2)/3
3824 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.50 e Å3
0 restraintsΔρmin = 0.28 e Å3
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*/Ueq
N10.65529 (10)0.48178 (8)0.34812 (10)0.0194 (2)
C20.52647 (12)0.48180 (10)0.33952 (12)0.0201 (2)
N30.45331 (10)0.40107 (9)0.37626 (10)0.0202 (2)
C40.52439 (11)0.31237 (10)0.43172 (11)0.0174 (2)
C50.65826 (11)0.30473 (10)0.44880 (11)0.0177 (2)
C60.72651 (11)0.39319 (10)0.40407 (11)0.0166 (2)
N70.69863 (10)0.20375 (9)0.50824 (11)0.0226 (2)
C80.58682 (13)0.15782 (11)0.52278 (13)0.0240 (3)
H10.5875 (16)0.0875 (15)0.5613 (15)0.029*
N90.47730 (10)0.21741 (9)0.47850 (11)0.0221 (2)
N20.46179 (13)0.57347 (11)0.28021 (13)0.0318 (3)
H20.3814 (19)0.5845 (16)0.2905 (17)0.038*
H30.5107 (19)0.6342 (17)0.2736 (17)0.038*
O10.85046 (8)0.39297 (7)0.41295 (8)0.01987 (18)
Na10.11614 (5)0.25458 (4)0.18294 (5)0.02088 (12)
Na20.04858 (5)0.04516 (4)0.37188 (5)0.02116 (12)
O2W0.30801 (10)0.32568 (9)0.13493 (10)0.0258 (2)
H40.3522 (18)0.3064 (15)0.0920 (17)0.031*
H50.3593 (18)0.3403 (15)0.2028 (18)0.031*
O3W0.18537 (10)0.38007 (8)0.35511 (9)0.0242 (2)
H60.1495 (17)0.4417 (16)0.3538 (16)0.029*
H70.2651 (18)0.3933 (15)0.3751 (16)0.029*
O4W0.24367 (9)0.11467 (8)0.31930 (9)0.0225 (2)
H80.2771 (17)0.0763 (15)0.2725 (16)0.027*
H90.3060 (18)0.1391 (15)0.3649 (16)0.027*
O5W0.00162 (10)0.06884 (8)0.14489 (9)0.02162 (19)
H100.0512 (17)0.0206 (15)0.1252 (15)0.026*
H110.0473 (18)0.0857 (15)0.0840 (17)0.026*
O6W0.15475 (10)0.02081 (9)0.42399 (10)0.0256 (2)
H120.2055 (18)0.0316 (16)0.4076 (16)0.031*
H130.1994 (17)0.0778 (16)0.4393 (16)0.031*
O7W0.04288 (10)0.22693 (8)0.46190 (9)0.0230 (2)
H140.0267 (18)0.2647 (15)0.4478 (16)0.028*
H150.0929 (17)0.2689 (15)0.4387 (16)0.028*
O8W0.08244 (9)0.15000 (8)0.31563 (9)0.02082 (19)
H160.1072 (16)0.1464 (14)0.2539 (17)0.025*
H170.1461 (17)0.1719 (14)0.3677 (16)0.025*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0164 (5)0.0202 (4)0.0221 (5)0.0017 (4)0.0046 (4)0.0029 (4)
C20.0178 (6)0.0207 (5)0.0207 (6)0.0009 (4)0.0016 (5)0.0017 (4)
N30.0137 (5)0.0228 (5)0.0237 (6)0.0005 (4)0.0025 (4)0.0024 (4)
C40.0134 (5)0.0211 (5)0.0176 (6)0.0015 (4)0.0030 (4)0.0008 (4)
C50.0127 (5)0.0200 (5)0.0201 (6)0.0007 (4)0.0025 (4)0.0024 (4)
C60.0141 (5)0.0203 (5)0.0154 (6)0.0010 (4)0.0033 (4)0.0012 (4)
N70.0180 (5)0.0221 (5)0.0274 (6)0.0027 (4)0.0036 (4)0.0061 (4)
C80.0201 (6)0.0233 (6)0.0288 (7)0.0000 (5)0.0050 (5)0.0052 (5)
N90.0161 (5)0.0232 (5)0.0272 (6)0.0011 (4)0.0052 (4)0.0037 (4)
N20.0221 (6)0.0274 (6)0.0454 (8)0.0054 (5)0.0059 (5)0.0139 (5)
O10.0112 (4)0.0256 (4)0.0230 (5)0.0017 (3)0.0040 (3)0.0006 (3)
Na10.0195 (3)0.0208 (2)0.0223 (3)0.00079 (18)0.0041 (2)0.00001 (19)
Na20.0223 (3)0.0199 (2)0.0225 (3)0.00009 (18)0.0076 (2)0.00032 (19)
O2W0.0206 (5)0.0346 (5)0.0237 (5)0.0011 (4)0.0080 (4)0.0038 (4)
O3W0.0163 (5)0.0230 (4)0.0339 (6)0.0007 (3)0.0064 (4)0.0032 (4)
O4W0.0169 (4)0.0261 (4)0.0249 (5)0.0005 (3)0.0052 (4)0.0061 (4)
O5W0.0226 (5)0.0218 (4)0.0194 (5)0.0038 (3)0.0014 (4)0.0008 (4)
O6W0.0206 (5)0.0231 (4)0.0342 (6)0.0009 (4)0.0083 (4)0.0048 (4)
O7W0.0227 (5)0.0210 (4)0.0264 (5)0.0033 (3)0.0076 (4)0.0007 (4)
O8W0.0175 (4)0.0265 (4)0.0180 (5)0.0009 (3)0.0025 (4)0.0025 (3)
Geometric parameters (Å, º) top
N1—C21.3419 (16)Na1—Na2ii4.1508 (7)
N1—C61.3596 (16)Na2—O6W2.3489 (11)
C2—N31.3371 (15)Na2—O7W2.3646 (10)
C2—N21.3720 (17)Na2—O4W2.3928 (10)
N3—C41.3581 (16)Na2—O8W2.4190 (10)
C4—N91.3660 (15)Na2—O6Wiii2.4661 (12)
C4—C51.3886 (16)Na2—O5W2.5133 (11)
C5—N71.3838 (15)Na2—Na2iii3.4096 (10)
C5—C61.4105 (15)O2W—H40.768 (19)
C6—O11.2903 (14)O2W—H50.86 (2)
N7—C81.3350 (16)O3W—H60.814 (18)
C8—N91.3561 (17)O3W—H70.840 (19)
C8—H10.931 (17)O4W—H80.823 (18)
N2—H20.89 (2)O4W—H90.801 (19)
N2—H30.89 (2)O5W—H100.853 (18)
Na1—O2W2.3474 (11)O5W—H110.779 (19)
Na1—O8Wi2.3762 (10)O6W—H120.81 (2)
Na1—O3W2.4233 (11)O6W—H130.854 (19)
Na1—O4W2.4539 (11)O7W—H140.844 (19)
Na1—O7Wii2.4577 (11)O7W—H150.802 (18)
Na1—O5W2.5008 (10)O8W—H160.789 (18)
Na1—Na23.4118 (7)O8W—H170.838 (18)
Na1—Na2i3.8174 (7)
C2—N1—C6119.40 (10)O4W—Na2—O5W74.31 (4)
N3—C2—N1127.97 (11)O8W—Na2—O5W81.48 (4)
N3—C2—N2116.29 (12)O6Wiii—Na2—O5W160.41 (4)
N1—C2—N2115.65 (11)O6W—Na2—Na2iii46.33 (3)
C2—N3—C4112.59 (10)O7W—Na2—Na2iii83.20 (3)
N3—C4—N9126.23 (11)O4W—Na2—Na2iii137.02 (4)
N3—C4—C5124.42 (11)O8W—Na2—Na2iii90.66 (3)
N9—C4—C5109.36 (11)O6Wiii—Na2—Na2iii43.55 (3)
N7—C5—C4109.15 (10)O5W—Na2—Na2iii148.46 (4)
N7—C5—C6132.17 (11)O6W—Na2—Na1123.80 (3)
C4—C5—C6118.67 (11)O7W—Na2—Na169.11 (3)
O1—C6—N1119.63 (10)O4W—Na2—Na145.99 (3)
O1—C6—C5123.46 (11)O8W—Na2—Na1117.28 (3)
N1—C6—C5116.90 (10)O6Wiii—Na2—Na1133.74 (3)
C8—N7—C5102.13 (10)O5W—Na2—Na146.97 (2)
N7—C8—N9117.07 (11)Na2iii—Na2—Na1152.06 (2)
N7—C8—H1119.3 (10)O6W—Na2—Na1iv61.54 (3)
N9—C8—H1123.6 (10)O7W—Na2—Na1iv145.46 (3)
C8—N9—C4102.30 (10)O4W—Na2—Na1iv130.52 (3)
C2—N2—H2116.5 (12)O8W—Na2—Na1iv36.85 (2)
C2—N2—H3115.3 (12)O6Wiii—Na2—Na1iv88.71 (3)
H2—N2—H3118.6 (17)O5W—Na2—Na1iv86.45 (3)
O2W—Na1—O8Wi129.40 (4)Na2iii—Na2—Na1iv69.845 (17)
O2W—Na1—O3W80.30 (4)Na1—Na2—Na1iv133.359 (16)
O8Wi—Na1—O3W80.46 (4)O6W—Na2—Na1v82.59 (3)
O2W—Na1—O4W89.48 (4)O7W—Na2—Na1v31.26 (3)
O8Wi—Na1—O4W133.17 (4)O4W—Na2—Na1v90.19 (3)
O3W—Na1—O4W82.39 (4)O8W—Na2—Na1v138.19 (3)
O2W—Na1—O7Wii81.27 (4)O6Wiii—Na2—Na1v54.92 (3)
O8Wi—Na1—O7Wii82.27 (4)O5W—Na2—Na1v139.21 (3)
O3W—Na1—O7Wii137.41 (4)Na2iii—Na2—Na1v59.699 (16)
O4W—Na1—O7Wii135.39 (4)Na1—Na2—Na1v95.407 (12)
O2W—Na1—O5W133.71 (4)Na1iv—Na2—Na1v129.544 (14)
O8Wi—Na1—O5W90.19 (4)Na1—O2W—H4134.3 (13)
O3W—Na1—O5W136.49 (4)Na1—O2W—H5106.6 (12)
O4W—Na1—O5W73.50 (4)H4—O2W—H5105.3 (18)
O7Wii—Na1—O5W81.89 (3)Na1—O3W—H6117.3 (13)
O2W—Na1—Na2134.00 (3)Na1—O3W—H7116.9 (12)
O8Wi—Na1—Na292.36 (3)H6—O3W—H7106.0 (17)
O3W—Na1—Na290.44 (3)Na2—O4W—Na189.48 (4)
O4W—Na1—Na244.53 (2)Na2—O4W—H8118.1 (12)
O7Wii—Na1—Na2128.98 (3)Na1—O4W—H8102.6 (12)
O5W—Na1—Na247.28 (3)Na2—O4W—H9126.8 (13)
O2W—Na1—Na2i91.78 (3)Na1—O4W—H9116.0 (12)
O8Wi—Na1—Na2i37.63 (2)H8—O4W—H9101.7 (17)
O3W—Na1—Na2i69.01 (3)Na1—O5W—Na285.75 (3)
O4W—Na1—Na2i150.71 (3)Na1—O5W—H10107.1 (11)
O7Wii—Na1—Na2i73.57 (3)Na2—O5W—H10100.0 (11)
O5W—Na1—Na2i123.73 (3)Na1—O5W—H1197.3 (13)
Na2—Na1—Na2i126.719 (14)Na2—O5W—H11152.4 (13)
O2W—Na1—Na2ii67.48 (3)H10—O5W—H11105.2 (17)
O8Wi—Na1—Na2ii74.69 (3)Na2—O6W—Na2iii90.13 (4)
O3W—Na1—Na2ii107.57 (3)Na2—O6W—H12129.0 (12)
O4W—Na1—Na2ii152.12 (3)Na2iii—O6W—H1297.4 (13)
O7Wii—Na1—Na2ii29.95 (2)Na2—O6W—H13121.5 (12)
O5W—Na1—Na2ii110.66 (3)Na2iii—O6W—H13102.9 (12)
Na2—Na1—Na2ii155.28 (2)H12—O6W—H13105.8 (17)
Na2i—Na1—Na2ii50.457 (14)Na2—O7W—Na1v118.79 (4)
O6W—Na2—O7W84.31 (4)Na2—O7W—H14119.2 (12)
O6W—Na2—O4W167.05 (4)Na1v—O7W—H14103.3 (12)
O7W—Na2—O4W83.97 (4)Na2—O7W—H15109.9 (12)
O6W—Na2—O8W98.02 (4)Na1v—O7W—H15100.4 (13)
O7W—Na2—O8W169.04 (4)H14—O7W—H15102.7 (17)
O4W—Na2—O8W94.52 (4)Na1iv—O8W—Na2105.52 (4)
O6W—Na2—O6Wiii89.87 (4)Na1iv—O8W—H16118.5 (12)
O7W—Na2—O6Wiii86.03 (4)Na2—O8W—H16105.7 (12)
O4W—Na2—O6Wiii94.77 (4)Na1iv—O8W—H17115.8 (11)
O8W—Na2—O6Wiii83.27 (4)Na2—O8W—H17104.3 (11)
O6W—Na2—O5W104.36 (4)H16—O8W—H17105.6 (17)
O7W—Na2—O5W108.41 (4)
C6—N1—C2—N32.7 (2)C2—N1—C6—C50.82 (17)
C6—N1—C2—N2179.09 (12)N7—C5—C6—O10.0 (2)
N1—C2—N3—C42.28 (19)C4—C5—C6—O1178.45 (11)
N2—C2—N3—C4178.68 (12)N7—C5—C6—N1179.41 (13)
C2—N3—C4—N9179.83 (12)C4—C5—C6—N10.95 (17)
C2—N3—C4—C50.21 (18)C4—C5—N7—C80.01 (14)
N3—C4—C5—N7179.91 (11)C6—C5—N7—C8178.58 (14)
N9—C4—C5—N70.41 (15)C5—N7—C8—N90.46 (16)
N3—C4—C5—C61.29 (19)N7—C8—N9—C40.70 (16)
N9—C4—C5—C6178.38 (11)N3—C4—N9—C8179.70 (12)
C2—N1—C6—O1179.76 (11)C5—C4—N9—C80.63 (14)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.86 (2)2.12 (2)2.9690 (16)167.5 (17)
O3W—H7···N30.840 (19)1.984 (19)2.7974 (14)163.0 (17)
O4W—H9···N90.801 (19)2.194 (19)2.9925 (15)175.1 (17)
O7W—H15···O3W0.802 (18)1.973 (19)2.7632 (13)168.3 (18)
O6W—H12···O2Wiv0.81 (2)2.00 (2)2.8026 (14)171.6 (18)
O3W—H6···O5Wi0.814 (18)2.159 (19)2.9410 (13)161.0 (17)
O2W—H4···N9ii0.768 (19)2.028 (19)2.7885 (14)170.7 (18)
O4W—H8···N1vi0.823 (18)1.989 (18)2.8098 (14)175.7 (17)
O5W—H10···O1vi0.853 (18)1.917 (18)2.7613 (12)170.2 (16)
O8W—H16···O1vi0.789 (18)2.063 (19)2.8401 (13)168.3 (17)
O5W—H11···O1vii0.779 (19)2.022 (19)2.7921 (14)169.7 (18)
O6W—H13···N7viii0.854 (19)2.066 (19)2.9098 (14)169.5 (17)
O7W—H14···O1viii0.844 (19)1.972 (19)2.7857 (13)161.6 (17)
O8W—H17···N7ix0.838 (18)1.962 (19)2.7953 (15)173.1 (16)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_250K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.564 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5440 (2) ÅCell parameters from 6590 reflections
b = 11.7396 (2) Åθ = 2.6–29.6°
c = 11.2426 (3) ŵ = 0.19 mm1
β = 101.476 (2)°T = 250 K
V = 1363.81 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3834 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus2965 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.047
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.806, Tmax = 1.000l = 1514
13095 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: difference Fourier map
wR(F2) = 0.096Only H-atom coordinates refined
S = 1.10 w = 1/[σ2(Fo2) + (0.0407P)2 + 0.5008P]
where P = (Fo2 + 2Fc2)/3
3834 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.43 e Å3
0 restraintsΔρmin = 0.22 e Å3
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*/Ueq
N10.65549 (11)0.48138 (9)0.34821 (11)0.0220 (2)
C20.52658 (13)0.48123 (11)0.33967 (13)0.0225 (3)
N30.45357 (10)0.40071 (9)0.37612 (11)0.0231 (2)
C40.52471 (12)0.31217 (10)0.43170 (12)0.0199 (2)
C50.65846 (12)0.30463 (10)0.44850 (12)0.0201 (2)
C60.72656 (12)0.39296 (10)0.40404 (11)0.0192 (2)
N70.69888 (11)0.20375 (9)0.50803 (11)0.0258 (2)
C80.58709 (13)0.15786 (12)0.52243 (14)0.0270 (3)
H10.5877 (17)0.0876 (16)0.5611 (16)0.032*
N90.47781 (11)0.21730 (10)0.47827 (11)0.0250 (2)
N20.46191 (14)0.57295 (12)0.28073 (14)0.0359 (3)
H20.378 (2)0.5834 (17)0.2913 (18)0.043*
H30.510 (2)0.6325 (18)0.2743 (18)0.043*
O10.85054 (9)0.39288 (8)0.41285 (9)0.0228 (2)
Na10.11637 (5)0.25468 (4)0.18273 (5)0.02402 (13)
Na20.04855 (5)0.04522 (4)0.37171 (5)0.02432 (13)
O2W0.30840 (10)0.32568 (9)0.13488 (11)0.0297 (2)
H40.3493 (19)0.3044 (16)0.0910 (19)0.036*
H50.3599 (19)0.3415 (16)0.2037 (19)0.036*
O3W0.18572 (10)0.38009 (9)0.35508 (10)0.0282 (2)
H60.1486 (18)0.4420 (16)0.3548 (17)0.034*
H70.265 (2)0.3927 (16)0.3755 (17)0.034*
O4W0.24383 (10)0.11463 (9)0.31907 (10)0.0258 (2)
H80.2775 (17)0.0755 (16)0.2728 (17)0.031*
H90.3055 (19)0.1399 (16)0.3650 (17)0.031*
O5W0.00130 (10)0.06896 (8)0.14477 (9)0.0248 (2)
H100.0482 (18)0.0212 (16)0.1257 (16)0.030*
H110.0464 (19)0.0857 (16)0.0848 (18)0.030*
O6W0.15473 (10)0.02076 (9)0.42402 (10)0.0292 (2)
H120.2055 (19)0.0307 (17)0.4081 (17)0.035*
H130.2002 (18)0.0773 (17)0.4390 (17)0.035*
O7W0.04299 (11)0.22684 (8)0.46171 (10)0.0263 (2)
H140.0264 (19)0.2632 (16)0.4474 (17)0.032*
H150.0927 (18)0.2697 (16)0.4370 (17)0.032*
O8W0.08234 (10)0.14992 (8)0.31554 (10)0.0240 (2)
H160.1083 (17)0.1460 (15)0.2513 (18)0.029*
H170.1432 (18)0.1714 (15)0.3663 (17)0.029*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0192 (5)0.0226 (5)0.0246 (6)0.0019 (4)0.0054 (4)0.0033 (4)
C20.0192 (6)0.0243 (6)0.0236 (7)0.0009 (5)0.0034 (5)0.0018 (5)
N30.0153 (5)0.0255 (5)0.0283 (6)0.0002 (4)0.0040 (4)0.0026 (4)
C40.0157 (6)0.0245 (6)0.0195 (6)0.0009 (4)0.0041 (5)0.0008 (5)
C50.0147 (6)0.0227 (5)0.0228 (7)0.0008 (4)0.0038 (5)0.0021 (5)
C60.0160 (6)0.0240 (5)0.0179 (6)0.0013 (4)0.0043 (5)0.0018 (4)
N70.0204 (5)0.0250 (5)0.0314 (7)0.0035 (4)0.0040 (5)0.0075 (5)
C80.0225 (7)0.0265 (6)0.0321 (8)0.0001 (5)0.0055 (6)0.0073 (5)
N90.0175 (5)0.0269 (5)0.0312 (7)0.0014 (4)0.0068 (5)0.0046 (5)
N20.0259 (7)0.0301 (6)0.0513 (9)0.0057 (5)0.0070 (6)0.0149 (6)
O10.0130 (4)0.0292 (4)0.0267 (5)0.0017 (3)0.0050 (4)0.0011 (4)
Na10.0219 (3)0.0244 (2)0.0259 (3)0.00082 (19)0.0050 (2)0.0000 (2)
Na20.0252 (3)0.0234 (2)0.0260 (3)0.0000 (2)0.0091 (2)0.0005 (2)
O2W0.0239 (5)0.0397 (5)0.0273 (6)0.0016 (4)0.0094 (4)0.0047 (4)
O3W0.0185 (5)0.0270 (5)0.0397 (6)0.0010 (4)0.0073 (4)0.0036 (4)
O4W0.0199 (5)0.0291 (5)0.0293 (6)0.0005 (4)0.0068 (4)0.0065 (4)
O5W0.0268 (5)0.0243 (4)0.0225 (5)0.0049 (4)0.0026 (4)0.0011 (4)
O6W0.0237 (5)0.0272 (5)0.0382 (6)0.0012 (4)0.0097 (4)0.0051 (4)
O7W0.0254 (5)0.0244 (4)0.0307 (6)0.0041 (4)0.0092 (4)0.0013 (4)
O8W0.0197 (5)0.0304 (5)0.0216 (5)0.0006 (4)0.0033 (4)0.0027 (4)
Geometric parameters (Å, º) top
N1—C21.3434 (17)Na1—Na2ii4.1547 (8)
N1—C61.3586 (17)Na2—O6W2.3504 (11)
C2—N31.3340 (16)Na2—O7W2.3658 (11)
C2—N21.3725 (18)Na2—O4W2.3955 (11)
N3—C41.3590 (16)Na2—O8W2.4214 (11)
C4—N91.3646 (16)Na2—O6Wiii2.4707 (13)
C4—C51.3880 (17)Na2—O5W2.5159 (12)
C5—N71.3851 (16)Na2—Na2iii3.4164 (10)
C5—C61.4085 (16)O2W—H40.76 (2)
C6—O11.2912 (15)O2W—H50.87 (2)
N7—C81.3347 (17)O3W—H60.82 (2)
C8—N91.3541 (18)O3W—H70.84 (2)
C8—H10.931 (18)O4W—H80.826 (19)
N2—H20.92 (2)O4W—H90.80 (2)
N2—H30.88 (2)O5W—H100.823 (19)
Na1—O2W2.3489 (11)O5W—H110.77 (2)
Na1—O8Wi2.3793 (11)O6W—H120.80 (2)
Na1—O3W2.4275 (12)O6W—H130.86 (2)
Na1—O4W2.4574 (12)O7W—H140.83 (2)
Na1—O7Wii2.4607 (12)O7W—H150.814 (19)
Na1—O5W2.5029 (11)O8W—H160.82 (2)
Na1—Na23.4171 (7)O8W—H170.809 (19)
Na1—Na2i3.8221 (7)
C2—N1—C6119.29 (11)O4W—Na2—O5W74.23 (4)
N3—C2—N1128.06 (12)O8W—Na2—O5W81.50 (4)
N3—C2—N2116.27 (12)O6Wiii—Na2—O5W160.38 (4)
N1—C2—N2115.59 (12)O6W—Na2—Na2iii46.32 (3)
C2—N3—C4112.57 (11)O7W—Na2—Na2iii83.22 (3)
N3—C4—N9126.28 (11)O4W—Na2—Na2iii136.97 (4)
N3—C4—C5124.35 (11)O8W—Na2—Na2iii90.61 (3)
N9—C4—C5109.37 (11)O6Wiii—Na2—Na2iii43.47 (3)
N7—C5—C4109.08 (11)O5W—Na2—Na2iii148.59 (4)
N7—C5—C6132.18 (12)O6W—Na2—Na1123.89 (3)
C4—C5—C6118.73 (11)O7W—Na2—Na169.11 (3)
O1—C6—N1119.54 (11)O4W—Na2—Na145.98 (3)
O1—C6—C5123.51 (12)O8W—Na2—Na1117.31 (3)
N1—C6—C5116.95 (11)O6Wiii—Na2—Na1133.74 (3)
C8—N7—C5102.09 (11)O5W—Na2—Na146.93 (3)
N7—C8—N9117.07 (12)Na2iii—Na2—Na1152.08 (3)
N7—C8—H1119.3 (11)O6W—Na2—Na1iv61.48 (3)
N9—C8—H1123.6 (11)O7W—Na2—Na1iv145.44 (3)
C8—N9—C4102.38 (11)O4W—Na2—Na1iv130.54 (3)
C2—N2—H2116.0 (13)O8W—Na2—Na1iv36.85 (3)
C2—N2—H3115.1 (13)O6Wiii—Na2—Na1iv88.66 (3)
H2—N2—H3119.4 (18)O5W—Na2—Na1iv86.55 (3)
O2W—Na1—O8Wi129.46 (4)Na2iii—Na2—Na1iv69.797 (18)
O2W—Na1—O3W80.28 (4)Na1—Na2—Na1iv133.426 (17)
O8Wi—Na1—O3W80.44 (4)O6W—Na2—Na1v82.61 (3)
O2W—Na1—O4W89.48 (4)O7W—Na2—Na1v31.27 (3)
O8Wi—Na1—O4W133.08 (4)O4W—Na2—Na1v90.18 (3)
O3W—Na1—O4W82.38 (4)O8W—Na2—Na1v138.14 (3)
O2W—Na1—O7Wii81.35 (4)O6Wiii—Na2—Na1v54.88 (3)
O8Wi—Na1—O7Wii82.32 (4)O5W—Na2—Na1v139.21 (3)
O3W—Na1—O7Wii137.46 (4)Na2iii—Na2—Na1v59.695 (17)
O4W—Na1—O7Wii135.39 (4)Na1—Na2—Na1v95.403 (12)
O2W—Na1—O5W133.69 (4)Na1iv—Na2—Na1v129.492 (15)
O8Wi—Na1—O5W90.23 (4)Na1—O2W—H4131.2 (15)
O3W—Na1—O5W136.45 (4)Na1—O2W—H5106.6 (13)
O4W—Na1—O5W73.41 (4)H4—O2W—H5108.2 (19)
O7Wii—Na1—O5W81.89 (4)Na1—O3W—H6117.6 (13)
O2W—Na1—Na2133.97 (4)Na1—O3W—H7116.9 (13)
O8Wi—Na1—Na292.30 (3)H6—O3W—H7107.1 (18)
O3W—Na1—Na290.41 (3)Na2—O4W—Na189.51 (4)
O4W—Na1—Na244.51 (3)Na2—O4W—H8117.7 (12)
O7Wii—Na1—Na2128.95 (3)Na1—O4W—H8103.3 (13)
O5W—Na1—Na247.25 (3)Na2—O4W—H9126.4 (13)
O2W—Na1—Na2i91.84 (3)Na1—O4W—H9115.2 (13)
O8Wi—Na1—Na2i37.62 (3)H8—O4W—H9102.4 (18)
O3W—Na1—Na2i69.01 (3)Na1—O5W—Na285.82 (4)
O4W—Na1—Na2i150.68 (3)Na1—O5W—H10108.7 (13)
O7Wii—Na1—Na2i73.62 (3)Na2—O5W—H10100.0 (13)
O5W—Na1—Na2i123.76 (3)Na1—O5W—H1197.2 (14)
Na2—Na1—Na2i126.649 (15)Na2—O5W—H11152.3 (14)
O2W—Na1—Na2ii67.57 (3)H10—O5W—H11105.0 (19)
O8Wi—Na1—Na2ii74.71 (3)Na2—O6W—Na2iii90.21 (4)
O3W—Na1—Na2ii107.63 (3)Na2—O6W—H12129.5 (13)
O4W—Na1—Na2ii152.18 (3)Na2iii—O6W—H1297.5 (13)
O7Wii—Na1—Na2ii29.93 (2)Na2—O6W—H13122.0 (12)
O5W—Na1—Na2ii110.64 (3)Na2iii—O6W—H13103.2 (13)
Na2—Na1—Na2ii155.22 (2)H12—O6W—H13104.7 (18)
Na2i—Na1—Na2ii50.508 (15)Na2—O7W—Na1v118.80 (5)
O6W—Na2—O7W84.36 (4)Na2—O7W—H14118.3 (13)
O6W—Na2—O4W167.12 (4)Na1v—O7W—H14103.7 (13)
O7W—Na2—O4W83.96 (4)Na2—O7W—H15109.8 (13)
O6W—Na2—O8W97.96 (4)Na1v—O7W—H15101.3 (13)
O7W—Na2—O8W169.01 (5)H14—O7W—H15102.6 (18)
O4W—Na2—O8W94.53 (4)Na1iv—O8W—Na2105.53 (4)
O6W—Na2—O6Wiii89.79 (4)Na1iv—O8W—H16118.7 (12)
O7W—Na2—O6Wiii86.00 (4)Na2—O8W—H16105.6 (12)
O4W—Na2—O6Wiii94.79 (4)Na1iv—O8W—H17115.0 (13)
O8W—Na2—O6Wiii83.27 (4)Na2—O8W—H17104.3 (13)
O6W—Na2—O5W104.50 (4)H16—O8W—H17106.3 (17)
O7W—Na2—O5W108.42 (4)
C6—N1—C2—N32.8 (2)C2—N1—C6—C50.90 (18)
C6—N1—C2—N2179.26 (13)N7—C5—C6—O10.2 (2)
N1—C2—N3—C42.5 (2)C4—C5—C6—O1178.54 (12)
N2—C2—N3—C4178.94 (13)N7—C5—C6—N1179.53 (13)
C2—N3—C4—N9179.81 (13)C4—C5—C6—N10.76 (18)
C2—N3—C4—C50.50 (19)C4—C5—N7—C80.17 (15)
N3—C4—C5—N7179.98 (12)C6—C5—N7—C8178.68 (15)
N9—C4—C5—N70.61 (16)C5—N7—C8—N90.35 (17)
N3—C4—C5—C61.0 (2)N7—C8—N9—C40.71 (18)
N9—C4—C5—C6178.42 (12)N3—C4—N9—C8179.85 (13)
C2—N1—C6—O1179.77 (12)C5—C4—N9—C80.76 (15)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.87 (2)2.11 (2)2.9703 (17)168.5 (18)
O3W—H7···N30.84 (2)1.98 (2)2.7973 (15)162.8 (18)
O4W—H9···N90.80 (2)2.20 (2)2.9977 (16)175.4 (18)
O7W—H15···O3W0.814 (19)1.96 (2)2.7671 (14)169.8 (19)
O6W—H12···O2Wiv0.80 (2)2.01 (2)2.8074 (16)171.0 (19)
O3W—H6···O5Wi0.82 (2)2.15 (2)2.9494 (14)162.1 (17)
O2W—H4···N9ii0.76 (2)2.05 (2)2.7922 (15)167 (2)
O4W—H8···N1vi0.826 (19)1.988 (19)2.8115 (15)175.2 (18)
O5W—H10···O1vi0.823 (19)1.94 (2)2.7621 (13)172.2 (18)
O8W—H16···O1vi0.82 (2)2.03 (2)2.8407 (14)168.2 (17)
O5W—H11···O1vii0.77 (2)2.04 (2)2.7962 (15)169.7 (19)
O6W—H13···N7viii0.86 (2)2.07 (2)2.9102 (15)169.4 (18)
O7W—H14···O1viii0.83 (2)1.99 (2)2.7884 (14)160.5 (18)
O8W—H17···N7ix0.809 (19)1.99 (2)2.7990 (16)172.7 (18)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_275K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.559 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5488 (2) ÅCell parameters from 5541 reflections
b = 11.7577 (2) Åθ = 2.5–29.6°
c = 11.2563 (3) ŵ = 0.19 mm1
β = 101.456 (2)°T = 275 K
V = 1368.31 (5) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3846 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus2961 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.044
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.890, Tmax = 1.000l = 1514
12706 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: difference Fourier map
wR(F2) = 0.112Only H-atom coordinates refined
S = 1.10 w = 1/[σ2(Fo2) + (0.0511P)2 + 0.5266P]
where P = (Fo2 + 2Fc2)/3
3846 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.41 e Å3
0 restraintsΔρmin = 0.23 e Å3
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*/Ueq
N10.65572 (12)0.48112 (10)0.34813 (12)0.0239 (2)
C20.52676 (14)0.48092 (12)0.33987 (14)0.0244 (3)
N30.45403 (11)0.40018 (10)0.37610 (12)0.0254 (3)
C40.52497 (13)0.31171 (11)0.43156 (13)0.0211 (3)
C50.65872 (13)0.30445 (11)0.44840 (13)0.0217 (3)
C60.72649 (13)0.39271 (11)0.40379 (12)0.0205 (3)
N70.69922 (12)0.20379 (10)0.50771 (12)0.0276 (3)
C80.58747 (15)0.15792 (13)0.52202 (16)0.0298 (3)
H10.5873 (19)0.0885 (17)0.5609 (18)0.036*
N90.47819 (12)0.21693 (11)0.47807 (13)0.0274 (3)
N20.46217 (15)0.57265 (13)0.28142 (16)0.0390 (4)
H20.379 (2)0.5812 (19)0.288 (2)0.047*
H30.512 (2)0.634 (2)0.273 (2)0.047*
O10.85067 (9)0.39275 (9)0.41288 (10)0.0251 (2)
Na10.11650 (6)0.25475 (5)0.18257 (6)0.02641 (15)
Na20.04863 (6)0.04523 (5)0.37154 (6)0.02681 (15)
O2W0.30862 (11)0.32546 (11)0.13466 (12)0.0322 (3)
H40.354 (2)0.3056 (18)0.090 (2)0.039*
H50.362 (2)0.3387 (18)0.204 (2)0.039*
O3W0.18630 (11)0.38023 (10)0.35523 (12)0.0315 (3)
H60.147 (2)0.4424 (18)0.3550 (19)0.038*
H70.269 (2)0.3925 (17)0.3772 (19)0.038*
O4W0.24399 (11)0.11469 (10)0.31903 (11)0.0287 (2)
H80.278 (2)0.0743 (18)0.2750 (19)0.034*
H90.308 (2)0.1403 (18)0.3632 (19)0.034*
O5W0.00100 (12)0.06912 (9)0.14484 (10)0.0277 (2)
H100.048 (2)0.0229 (18)0.1247 (18)0.033*
H110.044 (2)0.0865 (18)0.084 (2)0.033*
O6W0.15477 (11)0.02057 (10)0.42390 (11)0.0322 (3)
H120.208 (2)0.0315 (19)0.4077 (19)0.039*
H130.201 (2)0.0779 (19)0.4383 (19)0.039*
O7W0.04279 (12)0.22693 (9)0.46126 (11)0.0286 (2)
H140.029 (2)0.2639 (17)0.4460 (19)0.034*
H150.094 (2)0.2693 (18)0.4385 (19)0.034*
O8W0.08224 (11)0.14999 (9)0.31571 (11)0.0261 (2)
H160.1072 (19)0.1444 (16)0.251 (2)0.031*
H170.143 (2)0.1717 (17)0.3660 (19)0.031*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0211 (6)0.0249 (5)0.0262 (6)0.0026 (4)0.0056 (5)0.0038 (5)
C20.0215 (7)0.0254 (6)0.0259 (7)0.0023 (5)0.0039 (5)0.0024 (5)
N30.0175 (6)0.0275 (6)0.0312 (7)0.0003 (4)0.0046 (5)0.0033 (5)
C40.0153 (6)0.0257 (6)0.0222 (7)0.0017 (5)0.0034 (5)0.0006 (5)
C50.0154 (6)0.0249 (6)0.0244 (7)0.0009 (5)0.0031 (5)0.0029 (5)
C60.0168 (6)0.0250 (6)0.0200 (6)0.0019 (5)0.0039 (5)0.0022 (5)
N70.0209 (6)0.0276 (6)0.0338 (7)0.0033 (5)0.0041 (5)0.0077 (5)
C80.0248 (7)0.0281 (7)0.0362 (9)0.0005 (6)0.0057 (6)0.0087 (6)
N90.0204 (6)0.0283 (6)0.0343 (7)0.0016 (5)0.0076 (5)0.0055 (5)
N20.0256 (7)0.0339 (7)0.0563 (10)0.0062 (6)0.0055 (7)0.0168 (7)
O10.0149 (5)0.0314 (5)0.0296 (5)0.0022 (4)0.0056 (4)0.0017 (4)
Na10.0240 (3)0.0266 (3)0.0286 (3)0.0010 (2)0.0050 (2)0.0002 (2)
Na20.0283 (3)0.0251 (3)0.0289 (3)0.0000 (2)0.0104 (3)0.0003 (2)
O2W0.0242 (6)0.0436 (6)0.0302 (6)0.0015 (5)0.0090 (5)0.0043 (5)
O3W0.0203 (6)0.0302 (5)0.0448 (7)0.0016 (4)0.0082 (5)0.0033 (5)
O4W0.0217 (5)0.0314 (5)0.0340 (6)0.0002 (4)0.0075 (5)0.0071 (5)
O5W0.0312 (6)0.0267 (5)0.0245 (6)0.0055 (4)0.0037 (4)0.0015 (4)
O6W0.0257 (6)0.0299 (5)0.0425 (7)0.0005 (4)0.0105 (5)0.0057 (5)
O7W0.0262 (6)0.0266 (5)0.0342 (6)0.0040 (4)0.0089 (5)0.0010 (4)
O8W0.0212 (5)0.0325 (5)0.0242 (5)0.0007 (4)0.0034 (4)0.0035 (4)
Geometric parameters (Å, º) top
N1—C21.3450 (19)Na1—Na2ii4.1599 (8)
N1—C61.3581 (18)Na2—O6W2.3532 (13)
C2—N31.3343 (18)Na2—O7W2.3690 (12)
C2—N21.372 (2)Na2—O4W2.3974 (12)
N3—C41.3588 (18)Na2—O8W2.4245 (12)
C4—N91.3646 (17)Na2—O6Wiii2.4760 (14)
C4—C51.3884 (18)Na2—O5W2.5167 (13)
C5—N71.3840 (18)Na2—Na2iii3.4244 (12)
C5—C61.4081 (18)O2W—H40.80 (2)
C6—O11.2935 (16)O2W—H50.88 (2)
N7—C81.3349 (19)O3W—H60.84 (2)
C8—N91.352 (2)O3W—H70.87 (2)
C8—H10.93 (2)O4W—H80.82 (2)
N2—H20.90 (2)O4W—H90.81 (2)
N2—H30.91 (2)O5W—H100.82 (2)
Na1—O2W2.3503 (12)O5W—H110.77 (2)
Na1—O8Wi2.3803 (12)O6W—H120.82 (2)
Na1—O3W2.4347 (14)O6W—H130.86 (2)
Na1—O4W2.4617 (13)O7W—H140.86 (2)
Na1—O7Wii2.4673 (13)O7W—H150.81 (2)
Na1—O5W2.5043 (13)O8W—H160.82 (2)
Na1—Na23.4221 (8)O8W—H170.81 (2)
Na1—Na2i3.8274 (8)
C2—N1—C6119.10 (12)O4W—Na2—O5W74.21 (4)
N3—C2—N1127.96 (13)O8W—Na2—O5W81.63 (4)
N3—C2—N2116.42 (14)O6Wiii—Na2—O5W160.46 (5)
N1—C2—N2115.53 (13)O6W—Na2—Na1123.93 (4)
C2—N3—C4112.80 (12)O7W—Na2—Na169.03 (3)
N3—C4—N9126.40 (12)O4W—Na2—Na146.00 (3)
N3—C4—C5124.18 (12)O8W—Na2—Na1117.45 (3)
N9—C4—C5109.42 (12)O6Wiii—Na2—Na1133.73 (4)
N7—C5—C4109.05 (12)O5W—Na2—Na146.88 (3)
N7—C5—C6132.25 (13)O6W—Na2—Na2iii46.31 (3)
C4—C5—C6118.69 (12)O7W—Na2—Na2iii83.26 (4)
O1—C6—N1119.43 (12)O4W—Na2—Na2iii136.92 (5)
O1—C6—C5123.36 (13)O8W—Na2—Na2iii90.49 (4)
N1—C6—C5117.20 (12)O6Wiii—Na2—Na2iii43.41 (3)
C8—N7—C5102.03 (12)O5W—Na2—Na2iii148.66 (4)
N7—C8—N9117.23 (13)Na1—Na2—Na2iii152.05 (3)
N7—C8—H1119.8 (12)O6W—Na2—Na1iv61.39 (3)
N9—C8—H1122.9 (12)O7W—Na2—Na1iv145.39 (4)
C8—N9—C4102.26 (12)O4W—Na2—Na1iv130.62 (3)
C2—N2—H2116.5 (15)O8W—Na2—Na1iv36.80 (3)
C2—N2—H3115.6 (15)O6Wiii—Na2—Na1iv88.66 (3)
H2—N2—H3121 (2)O5W—Na2—Na1iv86.66 (3)
O2W—Na1—O8Wi129.53 (5)Na1—Na2—Na1iv133.492 (19)
O2W—Na1—O3W80.27 (5)Na2iii—Na2—Na1iv69.76 (2)
O8Wi—Na1—O3W80.54 (4)O6W—Na2—Na1v82.64 (4)
O2W—Na1—O4W89.47 (5)O7W—Na2—Na1v31.36 (3)
O8Wi—Na1—O4W133.05 (5)O4W—Na2—Na1v90.13 (3)
O3W—Na1—O4W82.31 (5)O8W—Na2—Na1v138.06 (4)
O2W—Na1—O7Wii81.41 (5)O6Wiii—Na2—Na1v54.80 (3)
O8Wi—Na1—O7Wii82.28 (4)O5W—Na2—Na1v139.17 (3)
O3W—Na1—O7Wii137.54 (5)Na1—Na2—Na1v95.387 (14)
O4W—Na1—O7Wii135.40 (5)Na2iii—Na2—Na1v59.680 (19)
O2W—Na1—O5W133.61 (5)Na1iv—Na2—Na1v129.437 (17)
O8Wi—Na1—O5W90.25 (4)Na1—O2W—H4133.9 (15)
O3W—Na1—O5W136.43 (5)Na1—O2W—H5106.8 (14)
O4W—Na1—O5W73.35 (4)H4—O2W—H5105 (2)
O7Wii—Na1—O5W81.88 (4)Na1—O3W—H6117.1 (15)
O2W—Na1—Na2133.92 (4)Na1—O3W—H7117.0 (14)
O8Wi—Na1—Na292.31 (3)H6—O3W—H7109 (2)
O3W—Na1—Na290.43 (3)Na2—O4W—Na189.53 (4)
O4W—Na1—Na244.47 (3)Na2—O4W—H8116.7 (14)
O7Wii—Na1—Na2128.87 (3)Na1—O4W—H8105.1 (14)
O5W—Na1—Na247.19 (3)Na2—O4W—H9128.7 (15)
O2W—Na1—Na2i91.93 (4)Na1—O4W—H9114.8 (15)
O8Wi—Na1—Na2i37.60 (3)H8—O4W—H9100 (2)
O3W—Na1—Na2i69.04 (3)Na1—O5W—Na285.93 (4)
O4W—Na1—Na2i150.60 (4)Na1—O5W—H10107.8 (14)
O7Wii—Na1—Na2i73.69 (3)Na2—O5W—H10101.0 (14)
O5W—Na1—Na2i123.81 (4)Na1—O5W—H1195.9 (16)
Na2—Na1—Na2i126.620 (17)Na2—O5W—H11154.2 (16)
O2W—Na1—Na2ii67.60 (4)H10—O5W—H11103 (2)
O8Wi—Na1—Na2ii74.71 (3)Na2—O6W—Na2iii90.29 (5)
O3W—Na1—Na2ii107.67 (4)Na2—O6W—H12130.2 (15)
O4W—Na1—Na2ii152.22 (3)Na2iii—O6W—H1297.7 (15)
O7Wii—Na1—Na2ii29.98 (3)Na2—O6W—H13121.6 (14)
O5W—Na1—Na2ii110.69 (3)Na2iii—O6W—H13103.6 (14)
Na2—Na1—Na2ii155.20 (3)H12—O6W—H13104 (2)
Na2i—Na1—Na2ii50.564 (17)Na2—O7W—Na1v118.65 (5)
O6W—Na2—O7W84.38 (5)Na2—O7W—H14117.8 (14)
O6W—Na2—O4W167.15 (5)Na1v—O7W—H14104.2 (14)
O7W—Na2—O4W83.93 (4)Na2—O7W—H15110.0 (14)
O6W—Na2—O8W97.81 (4)Na1v—O7W—H1599.7 (15)
O7W—Na2—O8W169.05 (5)H14—O7W—H15104 (2)
O4W—Na2—O8W94.67 (4)Na1iv—O8W—Na2105.60 (4)
O6W—Na2—O6Wiii89.71 (5)Na1iv—O8W—H16118.8 (14)
O7W—Na2—O6Wiii86.02 (4)Na2—O8W—H16104.0 (14)
O4W—Na2—O6Wiii94.80 (5)Na1iv—O8W—H17114.9 (14)
O8W—Na2—O6Wiii83.27 (4)Na2—O8W—H17104.7 (14)
O6W—Na2—O5W104.55 (5)H16—O8W—H17107.4 (19)
O7W—Na2—O5W108.29 (4)
C6—N1—C2—N33.0 (2)C2—N1—C6—C50.9 (2)
C6—N1—C2—N2179.43 (14)N7—C5—C6—O10.1 (3)
N1—C2—N3—C42.7 (2)C4—C5—C6—O1178.63 (13)
N2—C2—N3—C4179.13 (14)N7—C5—C6—N1179.50 (15)
C2—N3—C4—N9179.97 (14)C4—C5—C6—N11.0 (2)
C2—N3—C4—C50.5 (2)C4—C5—N7—C80.09 (17)
N3—C4—C5—N7179.97 (13)C6—C5—N7—C8178.53 (16)
N9—C4—C5—N70.52 (17)C5—N7—C8—N90.39 (19)
N3—C4—C5—C61.2 (2)N7—C8—N9—C40.7 (2)
N9—C4—C5—C6178.32 (13)N3—C4—N9—C8179.81 (14)
C2—N1—C6—O1179.48 (13)C5—C4—N9—C80.69 (17)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.88 (2)2.12 (2)2.9757 (19)166 (2)
O3W—H7···N30.87 (2)1.96 (2)2.7970 (16)162 (2)
O4W—H9···N90.81 (2)2.19 (2)2.9994 (18)177 (2)
O7W—H15···O3W0.81 (2)1.97 (2)2.7718 (16)168 (2)
O6W—H12···O2Wiv0.82 (2)2.00 (2)2.8118 (17)170 (2)
O3W—H6···O5Wi0.84 (2)2.15 (2)2.9585 (16)163 (2)
O2W—H4···N9ii0.80 (2)2.01 (2)2.7941 (17)170 (2)
O4W—H8···N1vi0.82 (2)2.00 (2)2.8137 (16)174 (2)
O5W—H10···O1vi0.82 (2)1.96 (2)2.7652 (15)170 (2)
O8W—H16···O1vi0.82 (2)2.03 (2)2.8456 (16)170.4 (19)
O5W—H11···O1vii0.77 (2)2.04 (2)2.8007 (16)171 (2)
O6W—H13···N7viii0.86 (2)2.06 (2)2.9120 (17)169 (2)
O7W—H14···O1viii0.86 (2)1.96 (2)2.7869 (15)159.5 (19)
O8W—H17···N7ix0.81 (2)2.00 (2)2.8010 (17)172 (2)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
disodium 2-amino-6-oxo-6,7-dihydro-1H-purine-1,7-diide heptahydrate (GuaNa_298K) top
Crystal data top
2(Na)·7(H2O)·C5H3N5OF(000) = 672
Mr = 321.21Dx = 1.554 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.5530 (2) ÅCell parameters from 5377 reflections
b = 11.7759 (2) Åθ = 2.4–29.6°
c = 11.2683 (3) ŵ = 0.19 mm1
β = 101.410 (2)°T = 298 K
V = 1372.65 (6) Å3Prism, colourless
Z = 40.5 × 0.5 × 0.25 mm
Data collection top
STOE IPDS 2
diffractometer
3857 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus2924 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.040
Detector resolution: 6.67 pixels mm-1θmax = 29.6°, θmin = 2.0°
rotation method scansh = 1414
Absorption correction: multi-scan
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1616
Tmin = 0.860, Tmax = 1.000l = 1514
12562 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: difference Fourier map
wR(F2) = 0.097Only H-atom coordinates refined
S = 1.05 w = 1/[σ2(Fo2) + (0.0431P)2 + 0.476P]
where P = (Fo2 + 2Fc2)/3
3857 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.23 e Å3
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*/Ueq
N10.65575 (11)0.48069 (9)0.34814 (11)0.0257 (2)
C20.52688 (13)0.48031 (11)0.33985 (13)0.0265 (3)
N30.45435 (10)0.39968 (9)0.37605 (11)0.0272 (2)
C40.52534 (12)0.31142 (10)0.43134 (12)0.0231 (2)
C50.65908 (12)0.30410 (10)0.44816 (12)0.0233 (2)
C60.72674 (11)0.39249 (10)0.40384 (11)0.0221 (2)
N70.69950 (11)0.20369 (10)0.50736 (11)0.0303 (3)
C80.58786 (14)0.15785 (12)0.52179 (14)0.0324 (3)
H10.5876 (17)0.0882 (16)0.5606 (16)0.039*
N90.47864 (11)0.21681 (10)0.47781 (11)0.0293 (3)
N20.46235 (14)0.57175 (12)0.28177 (15)0.0430 (3)
H20.382 (2)0.5820 (18)0.2930 (18)0.052*
H30.508 (2)0.6308 (19)0.2708 (19)0.052*
O10.85070 (8)0.39259 (8)0.41270 (9)0.0270 (2)
Na10.11673 (5)0.25483 (4)0.18243 (5)0.02906 (14)
Na20.04862 (5)0.04528 (4)0.37128 (5)0.02916 (14)
O2W0.30887 (11)0.32538 (10)0.13458 (11)0.0355 (2)
H40.3514 (19)0.3053 (16)0.0907 (19)0.043*
H50.3622 (19)0.3402 (16)0.2060 (19)0.043*
O3W0.18668 (11)0.38020 (9)0.35536 (11)0.0358 (2)
H60.1504 (19)0.4424 (17)0.3594 (18)0.043*
H70.266 (2)0.3934 (16)0.3792 (17)0.043*
O4W0.24435 (10)0.11458 (9)0.31885 (10)0.0310 (2)
H80.2771 (18)0.0744 (16)0.2722 (17)0.037*
H90.3051 (19)0.1403 (16)0.3623 (18)0.037*
O5W0.00050 (11)0.06935 (9)0.14478 (10)0.0306 (2)
H100.0504 (18)0.0227 (17)0.1257 (17)0.037*
H110.0431 (19)0.0863 (16)0.0861 (18)0.037*
O6W0.15465 (10)0.02060 (10)0.42385 (11)0.0355 (2)
H120.206 (2)0.0304 (18)0.4074 (18)0.043*
H130.1998 (19)0.0795 (17)0.4392 (17)0.043*
O7W0.04286 (11)0.22682 (9)0.46087 (10)0.0318 (2)
H140.0242 (19)0.2635 (16)0.4488 (17)0.038*
H150.0933 (18)0.2685 (16)0.4361 (17)0.038*
O8W0.08209 (10)0.15000 (9)0.31609 (10)0.0286 (2)
H160.1078 (17)0.1449 (15)0.2532 (18)0.034*
H170.1425 (18)0.1727 (15)0.3650 (17)0.034*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0216 (5)0.0268 (5)0.0288 (6)0.0023 (4)0.0056 (4)0.0037 (4)
C20.0228 (6)0.0276 (6)0.0285 (7)0.0021 (5)0.0035 (5)0.0030 (5)
N30.0177 (5)0.0297 (5)0.0340 (6)0.0003 (4)0.0044 (4)0.0040 (5)
C40.0172 (5)0.0281 (6)0.0238 (6)0.0016 (4)0.0039 (4)0.0006 (5)
C50.0163 (5)0.0270 (6)0.0262 (6)0.0011 (4)0.0034 (5)0.0031 (5)
C60.0164 (5)0.0277 (6)0.0221 (6)0.0019 (4)0.0038 (4)0.0022 (5)
N70.0226 (5)0.0303 (5)0.0374 (7)0.0032 (4)0.0045 (5)0.0087 (5)
C80.0260 (7)0.0318 (7)0.0396 (8)0.0004 (5)0.0070 (6)0.0091 (6)
N90.0201 (5)0.0310 (5)0.0372 (7)0.0016 (4)0.0070 (5)0.0065 (5)
N20.0309 (7)0.0356 (7)0.0624 (10)0.0075 (5)0.0087 (6)0.0182 (6)
O10.0149 (4)0.0346 (5)0.0320 (5)0.0024 (3)0.0055 (4)0.0017 (4)
Na10.0260 (3)0.0297 (3)0.0315 (3)0.0009 (2)0.0055 (2)0.0005 (2)
Na20.0299 (3)0.0278 (3)0.0318 (3)0.0001 (2)0.0110 (2)0.0003 (2)
O2W0.0273 (5)0.0485 (6)0.0324 (6)0.0019 (4)0.0103 (4)0.0051 (5)
O3W0.0227 (5)0.0333 (5)0.0524 (7)0.0012 (4)0.0098 (5)0.0042 (5)
O4W0.0230 (5)0.0356 (5)0.0352 (6)0.0007 (4)0.0074 (4)0.0078 (4)
O5W0.0328 (6)0.0297 (5)0.0281 (5)0.0060 (4)0.0032 (4)0.0019 (4)
O6W0.0277 (5)0.0331 (5)0.0472 (7)0.0014 (4)0.0113 (5)0.0071 (5)
O7W0.0301 (5)0.0292 (5)0.0376 (6)0.0051 (4)0.0106 (4)0.0011 (4)
O8W0.0234 (5)0.0358 (5)0.0262 (5)0.0014 (4)0.0038 (4)0.0038 (4)
Geometric parameters (Å, º) top
N1—C21.3446 (17)Na1—Na2ii4.1657 (8)
N1—C61.3593 (17)Na2—O6W2.3537 (12)
C2—N31.3331 (17)Na2—O7W2.3701 (11)
C2—N21.3693 (18)Na2—O4W2.4008 (11)
N3—C41.3584 (17)Na2—O8W2.4262 (11)
C4—N91.3640 (16)Na2—O6Wiii2.4822 (13)
C4—C51.3890 (16)Na2—O5W2.5178 (12)
C5—N71.3829 (16)Na2—Na2iii3.4328 (11)
C5—C61.4085 (16)O2W—H40.77 (2)
C6—O11.2921 (14)O2W—H50.90 (2)
N7—C81.3347 (17)O3W—H60.83 (2)
C8—N91.3529 (18)O3W—H70.84 (2)
C8—H10.930 (19)O4W—H80.832 (19)
N2—H20.89 (2)O4W—H90.79 (2)
N2—H30.87 (2)O5W—H100.83 (2)
Na1—O2W2.3505 (11)O5W—H110.75 (2)
Na1—O8Wi2.3816 (11)O6W—H120.81 (2)
Na1—O3W2.4398 (13)O6W—H130.88 (2)
Na1—O4W2.4669 (12)O7W—H140.82 (2)
Na1—O7Wii2.4732 (13)O7W—H150.81 (2)
Na1—O5W2.5047 (12)O8W—H160.81 (2)
Na1—Na23.4262 (8)O8W—H170.802 (19)
Na1—Na2i3.8330 (7)
C2—N1—C6119.14 (11)O4W—Na2—O5W74.16 (4)
N3—C2—N1127.96 (12)O8W—Na2—O5W81.84 (4)
N3—C2—N2116.42 (13)O6Wiii—Na2—O5W160.47 (4)
N1—C2—N2115.54 (12)O6W—Na2—Na1123.98 (4)
C2—N3—C4112.79 (11)O7W—Na2—Na168.97 (3)
N3—C4—N9126.35 (11)O4W—Na2—Na146.05 (3)
N3—C4—C5124.29 (11)O8W—Na2—Na1117.67 (3)
N9—C4—C5109.36 (11)O6Wiii—Na2—Na1133.74 (3)
N7—C5—C4109.08 (11)O5W—Na2—Na146.83 (3)
N7—C5—C6132.32 (11)O6W—Na2—Na2iii46.31 (3)
C4—C5—C6118.58 (11)O7W—Na2—Na2iii83.29 (3)
O1—C6—N1119.48 (11)O4W—Na2—Na2iii136.81 (4)
O1—C6—C5123.35 (12)O8W—Na2—Na2iii90.30 (3)
N1—C6—C5117.17 (11)O6Wiii—Na2—Na2iii43.28 (3)
C8—N7—C5102.07 (11)O5W—Na2—Na2iii148.82 (4)
N7—C8—N9117.15 (12)Na1—Na2—Na2iii152.02 (3)
N7—C8—H1120.0 (11)O6W—Na2—Na1iv61.34 (3)
N9—C8—H1122.9 (11)O7W—Na2—Na1iv145.37 (3)
C8—N9—C4102.33 (11)O4W—Na2—Na1iv130.65 (3)
C2—N2—H2115.9 (14)O8W—Na2—Na1iv36.73 (3)
C2—N2—H3117.5 (14)O6Wiii—Na2—Na1iv88.58 (3)
H2—N2—H3118.7 (19)O5W—Na2—Na1iv86.81 (3)
O2W—Na1—O8Wi129.52 (4)Na1—Na2—Na1iv133.589 (17)
O2W—Na1—O3W80.26 (4)Na2iii—Na2—Na1iv69.717 (18)
O8Wi—Na1—O3W80.65 (4)O6W—Na2—Na1v82.65 (3)
O2W—Na1—O4W89.44 (4)O7W—Na2—Na1v31.41 (3)
O8Wi—Na1—O4W133.14 (4)O4W—Na2—Na1v90.08 (3)
O3W—Na1—O4W82.29 (4)O8W—Na2—Na1v137.87 (3)
O2W—Na1—O7Wii81.46 (4)O6Wiii—Na2—Na1v54.75 (3)
O8Wi—Na1—O7Wii82.17 (4)O5W—Na2—Na1v139.13 (3)
O3W—Na1—O7Wii137.60 (4)Na1—Na2—Na1v95.356 (13)
O4W—Na1—O7Wii135.37 (4)Na2iii—Na2—Na1v59.663 (18)
O2W—Na1—O5W133.55 (4)Na1iv—Na2—Na1v129.379 (15)
O8Wi—Na1—O5W90.30 (4)Na1—O2W—H4132.8 (15)
O3W—Na1—O5W136.40 (4)Na1—O2W—H5106.1 (12)
O4W—Na1—O5W73.27 (4)H4—O2W—H5107.0 (19)
O7Wii—Na1—O5W81.88 (4)Na1—O3W—H6120.4 (14)
O2W—Na1—Na2133.91 (4)Na1—O3W—H7119.4 (13)
O8Wi—Na1—Na292.36 (3)H6—O3W—H7105.1 (18)
O3W—Na1—Na290.41 (3)Na2—O4W—Na189.47 (4)
O4W—Na1—Na244.48 (3)Na2—O4W—H8116.6 (12)
O7Wii—Na1—Na2128.82 (3)Na1—O4W—H8103.4 (13)
O5W—Na1—Na247.15 (3)Na2—O4W—H9127.8 (14)
O2W—Na1—Na2i91.99 (3)Na1—O4W—H9114.0 (14)
O8Wi—Na1—Na2i37.54 (3)H8—O4W—H9102.9 (18)
O3W—Na1—Na2i69.05 (3)Na1—O5W—Na286.03 (4)
O4W—Na1—Na2i150.59 (3)Na1—O5W—H10107.4 (13)
O7Wii—Na1—Na2i73.74 (3)Na2—O5W—H10100.1 (13)
O5W—Na1—Na2i123.87 (3)Na1—O5W—H1196.2 (15)
Na2—Na1—Na2i126.574 (16)Na2—O5W—H11153.1 (15)
O2W—Na1—Na2ii67.68 (3)H10—O5W—H11104.8 (19)
O8Wi—Na1—Na2ii74.60 (3)Na2—O6W—Na2iii90.41 (4)
O3W—Na1—Na2ii107.75 (3)Na2—O6W—H12129.9 (14)
O4W—Na1—Na2ii152.23 (3)Na2iii—O6W—H1298.1 (14)
O7Wii—Na1—Na2ii29.96 (3)Na2—O6W—H13120.6 (12)
O5W—Na1—Na2ii110.67 (3)Na2iii—O6W—H13103.0 (12)
Na2—Na1—Na2ii155.13 (2)H12—O6W—H13105.4 (18)
Na2i—Na1—Na2ii50.620 (15)Na2—O7W—Na1v118.64 (5)
O6W—Na2—O7W84.42 (4)Na2—O7W—H14120.0 (13)
O6W—Na2—O4W167.21 (4)Na1v—O7W—H14102.2 (13)
O7W—Na2—O4W83.92 (4)Na2—O7W—H15108.9 (13)
O6W—Na2—O8W97.68 (4)Na1v—O7W—H15101.3 (13)
O7W—Na2—O8W168.93 (5)H14—O7W—H15103.2 (18)
O4W—Na2—O8W94.77 (4)Na1iv—O8W—Na2105.73 (4)
O6W—Na2—O6Wiii89.59 (4)Na1iv—O8W—H16119.3 (13)
O7W—Na2—O6Wiii86.02 (4)Na2—O8W—H16104.2 (13)
O4W—Na2—O6Wiii94.80 (4)Na1iv—O8W—H17114.8 (13)
O8W—Na2—O6Wiii83.13 (4)Na2—O8W—H17106.0 (13)
O6W—Na2—O5W104.71 (4)H16—O8W—H17105.6 (18)
O7W—Na2—O5W108.23 (4)
C6—N1—C2—N33.0 (2)C2—N1—C6—C51.05 (18)
C6—N1—C2—N2179.58 (13)N7—C5—C6—O10.2 (2)
N1—C2—N3—C42.6 (2)C4—C5—C6—O1178.55 (12)
N2—C2—N3—C4179.19 (13)N7—C5—C6—N1179.53 (13)
C2—N3—C4—N9180.00 (13)C4—C5—C6—N10.74 (19)
C2—N3—C4—C50.53 (19)C4—C5—N7—C80.07 (15)
N3—C4—C5—N7179.92 (12)C6—C5—N7—C8178.80 (15)
N9—C4—C5—N70.54 (16)C5—N7—C8—N90.44 (18)
N3—C4—C5—C61.0 (2)N7—C8—N9—C40.76 (18)
N9—C4—C5—C6178.52 (12)N3—C4—N9—C8179.73 (13)
C2—N1—C6—O1179.64 (12)C5—C4—N9—C80.74 (16)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y, z+1; (iv) x, y1/2, z+1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2W—H5···N30.90 (2)2.09 (2)2.9789 (17)167.5 (17)
O3W—H7···N30.84 (2)1.99 (2)2.7974 (15)158.9 (18)
O4W—H9···N90.79 (2)2.22 (2)3.0031 (16)177.4 (19)
O7W—H15···O3W0.81 (2)1.97 (2)2.7736 (15)169.3 (19)
O6W—H12···O2Wiv0.81 (2)2.02 (2)2.8184 (16)170.3 (19)
O3W—H6···O5Wi0.83 (2)2.17 (2)2.9699 (15)161.2 (18)
O2W—H4···N9ii0.77 (2)2.04 (2)2.7981 (16)169 (2)
O4W—H8···N1vi0.832 (19)1.98 (2)2.8148 (15)175.9 (18)
O5W—H10···O1vi0.83 (2)1.95 (2)2.7671 (14)169.9 (18)
O8W—H16···O1vi0.81 (2)2.05 (2)2.8504 (14)169.4 (17)
O5W—H11···O1vii0.75 (2)2.07 (2)2.8073 (15)170 (2)
O6W—H13···N7viii0.88 (2)2.04 (2)2.9114 (16)169.1 (17)
O7W—H14···O1viii0.82 (2)2.00 (2)2.7896 (14)161.7 (18)
O8W—H17···N7ix0.802 (19)2.01 (2)2.8028 (16)171.0 (18)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iv) x, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x1, y+1/2, z1/2; (viii) x1, y, z; (ix) x+1, y, z+1.
 

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