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The title anion, (C7H8N5O4)−, L−, forms hydrated metal complexes with a range of metal ions M+ and M2+. Lithium and manganese(II) form finite molecular aggregates [Li(L)(H2O)3] (1) and [Mn(L)2(H2O)4].6H2O (4) in which the molecular aggregates are linked into three-dimensional frameworks by extensive hydrogen bonding. The sodium and potassium derivatives, [Na2(L)2(H2O)3] (2) and [K(L)(H2O)] (3) both form organic–inorganic hybrid sheets in which metal–oxygen ribbons are linked by strips containing only organic ligands: these sheets are linked by hydrogen bonds into three-dimensional frameworks. In (2) the metal–oxygen ribbon is built from pairs of edge-shared trigonal bipyramids linked by water molecules, while in (3) it consists of a continuous chain of vertex-sharing octahedra. The nitroso group in the anion acts as an η1 ligand towards Na+ and as an η2 ligand towards K+. In all cases the anion L− shows the same unusual pattern of interatomic distances as the neutral parent LH.
Supporting information
CCDC references: 166498; 166499; 166500; 166501
For all compounds, data collection: Kappa-CCD server software (Nonius, 1997); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b). Molecular graphics: PLATON (Spek, 2000) for (1); ORTEP (Johnson, 1976), PLATON (Spek, 2000) for 190, (3), MnL2. For all compounds, software used to prepare material for publication: SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).
(1) Triaqua-
N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidine-2-yl)
glycinatolithium,
top
Crystal data top
C7H14LiN5O7 | F(000) = 1200 |
Mr = 287.17 | Dx = 1.577 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 24.7736 (6) Å | Cell parameters from 2637 reflections |
b = 7.6525 (3) Å | θ = 3.0–27.5° |
c = 14.0096 (5) Å | µ = 0.14 mm−1 |
β = 114.3751 (13)° | T = 150 K |
V = 2419.20 (14) Å3 | Block, red |
Z = 8 | 0.20 × 0.10 × 0.10 mm |
Data collection top
Kappa-CCD diffractometer | 2637 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 2024 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ϕ scans and ω scans with κ offsets | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | h = −32→32 |
Tmin = 0.973, Tmax = 0.986 | k = −9→9 |
7232 measured reflections | l = −18→18 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.121 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0621P)2 + 0.6971P] where P = (Fo2 + 2Fc2)/3 |
2637 reflections | (Δ/σ)max = 0.001 |
200 parameters | Δρmax = 0.24 e Å−3 |
9 restraints | Δρmin = −0.30 e Å−3 |
Crystal data top
C7H14LiN5O7 | V = 2419.20 (14) Å3 |
Mr = 287.17 | Z = 8 |
Monoclinic, C2/c | Mo Kα radiation |
a = 24.7736 (6) Å | µ = 0.14 mm−1 |
b = 7.6525 (3) Å | T = 150 K |
c = 14.0096 (5) Å | 0.20 × 0.10 × 0.10 mm |
β = 114.3751 (13)° | |
Data collection top
Kappa-CCD diffractometer | 2637 independent reflections |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | 2024 reflections with I > 2σ(I) |
Tmin = 0.973, Tmax = 0.986 | Rint = 0.027 |
7232 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.045 | 9 restraints |
wR(F2) = 0.121 | H-atom parameters constrained |
S = 1.03 | Δρmax = 0.24 e Å−3 |
2637 reflections | Δρmin = −0.30 e Å−3 |
200 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Li1 | 0.29248 (13) | 0.3873 (4) | 0.1674 (2) | 0.0209 (6) | |
N1 | 0.44897 (6) | 0.77584 (19) | 0.11599 (12) | 0.0173 (3) | |
C2 | 0.42022 (7) | 0.9234 (2) | 0.11378 (13) | 0.0160 (4) | |
N2 | 0.36671 (6) | 0.91241 (19) | 0.11396 (11) | 0.0182 (3) | |
H2 | 0.3456 | 1.0081 | 0.1060 | 0.022* | |
C21 | 0.34233 (7) | 0.7469 (2) | 0.12697 (14) | 0.0187 (4) | |
H21A | 0.3121 | 0.7702 | 0.1546 | 0.022* | |
H21B | 0.3744 | 0.6783 | 0.1806 | 0.022* | |
C22 | 0.31410 (7) | 0.6355 (2) | 0.02917 (13) | 0.0152 (4) | |
O21 | 0.29906 (5) | 0.48528 (15) | 0.04541 (9) | 0.0188 (3) | |
O22 | 0.30629 (5) | 0.69571 (15) | −0.05865 (9) | 0.0202 (3) | |
N3 | 0.44254 (6) | 1.08863 (18) | 0.11320 (11) | 0.0165 (3) | |
C3 | 0.40555 (8) | 1.2438 (2) | 0.10341 (15) | 0.0230 (4) | |
H3A | 0.3670 | 1.2282 | 0.0443 | 0.034* | |
H3B | 0.4252 | 1.3472 | 0.0914 | 0.034* | |
H3C | 0.3998 | 1.2592 | 0.1681 | 0.034* | |
C4 | 0.50067 (7) | 1.1121 (2) | 0.12467 (13) | 0.0160 (4) | |
O4 | 0.52105 (5) | 1.25971 (15) | 0.13151 (10) | 0.0221 (3) | |
C5 | 0.53312 (7) | 0.9528 (2) | 0.12704 (13) | 0.0164 (4) | |
N5 | 0.58835 (6) | 0.98110 (19) | 0.13560 (11) | 0.0183 (3) | |
O5 | 0.61943 (5) | 0.84596 (16) | 0.13552 (10) | 0.0213 (3) | |
C6 | 0.50410 (7) | 0.7866 (2) | 0.12094 (13) | 0.0167 (4) | |
N6 | 0.53190 (6) | 0.63922 (19) | 0.12209 (11) | 0.0198 (3) | |
H6A | 0.5142 | 0.5385 | 0.1196 | 0.024* | |
H6B | 0.5681 | 0.6415 | 0.1253 | 0.024* | |
O1 | 0.35831 (5) | 0.39663 (16) | 0.30945 (9) | 0.0207 (3) | |
H11 | 0.3391 (7) | 0.383 (2) | 0.3560 (11) | 0.025* | |
H12 | 0.3898 (6) | 0.3123 (19) | 0.3294 (13) | 0.025* | |
O2 | 0.27923 (5) | 0.13984 (16) | 0.14011 (9) | 0.0198 (3) | |
H21 | 0.2744 (7) | 0.089 (2) | 0.1984 (7) | 0.024* | |
H22 | 0.2485 (6) | 0.096 (2) | 0.0771 (6) | 0.024* | |
O3 | 0.22339 (5) | 0.50360 (16) | 0.17302 (9) | 0.0198 (3) | |
H31 | 0.2134 (6) | 0.6065 (14) | 0.1305 (12) | 0.024* | |
H32 | 0.1875 (4) | 0.4410 (18) | 0.1594 (14) | 0.024* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Li1 | 0.0203 (14) | 0.0192 (15) | 0.0242 (16) | −0.0007 (12) | 0.0103 (13) | 0.0009 (13) |
N1 | 0.0143 (7) | 0.0166 (7) | 0.0201 (8) | −0.0010 (6) | 0.0061 (6) | 0.0003 (6) |
C2 | 0.0161 (8) | 0.0177 (8) | 0.0125 (9) | −0.0030 (7) | 0.0042 (7) | −0.0020 (7) |
N2 | 0.0154 (7) | 0.0176 (7) | 0.0211 (8) | −0.0013 (6) | 0.0072 (6) | −0.0018 (6) |
C21 | 0.0180 (8) | 0.0192 (9) | 0.0189 (10) | −0.0032 (7) | 0.0077 (7) | −0.0018 (7) |
C22 | 0.0112 (7) | 0.0166 (8) | 0.0188 (9) | 0.0023 (7) | 0.0074 (7) | 0.0003 (7) |
O21 | 0.0225 (6) | 0.0153 (6) | 0.0185 (7) | −0.0018 (5) | 0.0085 (5) | 0.0006 (5) |
O22 | 0.0243 (6) | 0.0200 (6) | 0.0171 (7) | 0.0009 (5) | 0.0094 (5) | 0.0025 (5) |
N3 | 0.0158 (7) | 0.0145 (7) | 0.0185 (8) | −0.0007 (6) | 0.0063 (6) | −0.0006 (6) |
C3 | 0.0229 (9) | 0.0158 (9) | 0.0312 (11) | 0.0013 (7) | 0.0120 (8) | −0.0004 (8) |
C4 | 0.0173 (8) | 0.0183 (9) | 0.0122 (9) | −0.0018 (7) | 0.0058 (7) | 0.0011 (7) |
O4 | 0.0223 (7) | 0.0155 (6) | 0.0289 (8) | −0.0032 (5) | 0.0109 (6) | −0.0004 (5) |
C5 | 0.0169 (8) | 0.0169 (8) | 0.0144 (9) | −0.0009 (7) | 0.0055 (7) | 0.0002 (7) |
N5 | 0.0161 (7) | 0.0209 (7) | 0.0171 (8) | 0.0006 (6) | 0.0062 (6) | 0.0019 (6) |
O5 | 0.0172 (6) | 0.0215 (6) | 0.0253 (7) | 0.0043 (5) | 0.0089 (5) | 0.0024 (5) |
C6 | 0.0174 (8) | 0.0183 (9) | 0.0122 (9) | 0.0001 (7) | 0.0039 (7) | 0.0003 (7) |
N6 | 0.0166 (7) | 0.0147 (7) | 0.0278 (9) | −0.0002 (6) | 0.0087 (7) | 0.0003 (6) |
O1 | 0.0182 (6) | 0.0239 (7) | 0.0204 (7) | 0.0014 (5) | 0.0083 (5) | 0.0017 (5) |
O2 | 0.0211 (6) | 0.0187 (6) | 0.0181 (7) | −0.0028 (5) | 0.0067 (5) | −0.0010 (5) |
O3 | 0.0181 (6) | 0.0187 (6) | 0.0232 (7) | 0.0009 (5) | 0.0092 (5) | 0.0031 (5) |
Geometric parameters (Å, º) top
Li1—O2 | 1.933 (3) | C3—H3A | 0.9800 |
Li1—O21 | 1.934 (3) | C3—H3B | 0.9800 |
Li1—O3 | 1.959 (3) | C3—H3C | 0.9800 |
Li1—O1 | 1.986 (3) | C4—O4 | 1.2248 (19) |
N1—C2 | 1.329 (2) | C4—C5 | 1.453 (2) |
N1—C6 | 1.341 (2) | C5—N5 | 1.341 (2) |
C2—N2 | 1.329 (2) | C5—C6 | 1.446 (2) |
C2—N3 | 1.381 (2) | N5—O5 | 1.2896 (19) |
N2—C21 | 1.447 (2) | C6—N6 | 1.318 (2) |
N2—H2 | 0.8800 | N6—H6A | 0.8800 |
C21—C22 | 1.517 (2) | N6—H6B | 0.8800 |
C21—H21A | 0.9900 | O1—H11 | 0.959 (17) |
C21—H21B | 0.9900 | O1—H12 | 0.961 (16) |
C22—O22 | 1.252 (2) | O2—H21 | 0.956 (13) |
C22—O21 | 1.258 (2) | O2—H22 | 0.957 (10) |
N3—C4 | 1.393 (2) | O3—H31 | 0.956 (12) |
N3—C3 | 1.471 (2) | O3—H32 | 0.957 (13) |
| | | |
O2—Li1—O21 | 105.91 (15) | N3—C3—H3B | 109.5 |
O2—Li1—O3 | 111.91 (14) | H3A—C3—H3B | 109.5 |
O21—Li1—O3 | 104.65 (14) | N3—C3—H3C | 109.5 |
O2—Li1—O1 | 103.63 (14) | H3A—C3—H3C | 109.5 |
O21—Li1—O1 | 122.51 (15) | H3B—C3—H3C | 109.5 |
O3—Li1—O1 | 108.26 (15) | O4—C4—N3 | 120.07 (15) |
C2—N1—C6 | 118.28 (14) | O4—C4—C5 | 124.45 (15) |
N1—C2—N2 | 118.14 (15) | N3—C4—C5 | 115.48 (14) |
N1—C2—N3 | 124.48 (15) | N5—C5—C6 | 127.70 (15) |
N2—C2—N3 | 117.38 (15) | N5—C5—C4 | 113.63 (14) |
C2—N2—C21 | 121.62 (14) | C6—C5—C4 | 118.67 (15) |
C2—N2—H2 | 119.2 | O5—N5—C5 | 117.25 (14) |
C21—N2—H2 | 119.2 | N6—C6—N1 | 117.64 (15) |
N2—C21—C22 | 116.04 (14) | N6—C6—C5 | 120.49 (15) |
N2—C21—H21A | 108.3 | N1—C6—C5 | 121.86 (15) |
C22—C21—H21A | 108.3 | C6—N6—H6A | 120.0 |
N2—C21—H21B | 108.3 | C6—N6—H6B | 120.0 |
C22—C21—H21B | 108.3 | H6A—N6—H6B | 120.0 |
H21A—C21—H21B | 107.4 | Li1—O1—H11 | 104.1 (11) |
O22—C22—O21 | 125.25 (15) | Li1—O1—H12 | 120.0 (11) |
O22—C22—C21 | 120.47 (15) | H11—O1—H12 | 107.5 (7) |
O21—C22—C21 | 114.26 (14) | Li1—O2—H21 | 107.5 (10) |
C22—O21—Li1 | 130.81 (14) | Li1—O2—H22 | 122.0 (11) |
C2—N3—C4 | 120.97 (14) | H21—O2—H22 | 108.2 (7) |
C2—N3—C3 | 120.25 (13) | Li1—O3—H31 | 110.8 (10) |
C4—N3—C3 | 118.76 (13) | Li1—O3—H32 | 121.3 (11) |
N3—C3—H3A | 109.5 | H31—O3—H32 | 107.9 (7) |
| | | |
C6—N1—C2—N2 | −176.83 (15) | C2—N3—C4—O4 | −174.77 (15) |
C6—N1—C2—N3 | 1.9 (3) | C3—N3—C4—O4 | 3.5 (2) |
N1—C2—N2—C21 | 6.2 (2) | C2—N3—C4—C5 | 5.5 (2) |
N3—C2—N2—C21 | −172.61 (15) | C3—N3—C4—C5 | −176.18 (14) |
C2—N2—C21—C22 | −81.9 (2) | O4—C4—C5—N5 | −1.2 (3) |
N2—C21—C22—O22 | −8.6 (2) | N3—C4—C5—N5 | 178.47 (14) |
N2—C21—C22—O21 | 172.84 (14) | O4—C4—C5—C6 | 178.40 (16) |
O22—C22—O21—Li1 | −165.69 (16) | N3—C4—C5—C6 | −1.9 (2) |
C21—C22—O21—Li1 | 12.8 (2) | C6—C5—N5—O5 | 2.2 (3) |
O2—Li1—O21—C22 | −171.10 (14) | C4—C5—N5—O5 | −178.28 (14) |
O3—Li1—O21—C22 | 70.5 (2) | C2—N1—C6—N6 | −179.38 (15) |
O1—Li1—O21—C22 | −52.9 (3) | C2—N1—C6—C5 | 1.9 (3) |
N1—C2—N3—C4 | −6.0 (3) | N5—C5—C6—N6 | −1.0 (3) |
N2—C2—N3—C4 | 172.82 (15) | C4—C5—C6—N6 | 179.51 (15) |
N1—C2—N3—C3 | 175.80 (16) | N5—C5—C6—N1 | 177.74 (16) |
N2—C2—N3—C3 | −5.4 (2) | C4—C5—C6—N1 | −1.8 (3) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O2i | 0.88 | 2.14 | 2.918 (2) | 146 |
N6—H6A···O4ii | 0.88 | 2.14 | 2.925 (2) | 148 |
N6—H6B···O1iii | 0.88 | 2.51 | 3.100 (2) | 125 |
O1—H11···O22iv | 0.96 (2) | 1.80 (2) | 2.746 (2) | 167 (1) |
O1—H12···O4v | 0.96 (2) | 2.08 (2) | 2.945 (2) | 148 (1) |
O2—H21···O3vi | 0.96 (1) | 1.90 (1) | 2.844 (2) | 171 (1) |
O2—H22···O21vii | 0.96 (1) | 1.75 (1) | 2.697 (2) | 171 (1) |
O3—H31···O22viii | 0.96 (1) | 1.77 (1) | 2.726 (2) | 176 (1) |
O3—H32···O5ix | 0.96 (1) | 1.74 (1) | 2.692 (2) | 175 (1) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x+1, y, −z+1/2; (iv) x, −y+1, z+1/2; (v) −x+1, y−1, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z; (viii) −x+1/2, −y+3/2, −z; (ix) x−1/2, y−1/2, z. |
(190) Triaqua-bis[
N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-
oxopyrimidin-2-yl)glycinato]disodium
top
Crystal data top
C14H22N10Na2O11 | Z = 2 |
Mr = 552.40 | F(000) = 572 |
Triclinic, P1 | Dx = 1.707 Mg m−3 |
a = 7.5702 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.5237 (2) Å | Cell parameters from 5449 reflections |
c = 13.3743 (3) Å | θ = 2.9–29.0° |
α = 104.4350 (8)° | µ = 0.18 mm−1 |
β = 97.8415 (8)° | T = 150 K |
γ = 103.5004 (7)° | Plate, colourless |
V = 1074.95 (3) Å3 | 0.45 × 0.25 × 0.05 mm |
Data collection top
Kappa-CCD diffractometer | 5449 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 4455 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
ϕ scans and ω scans with κ offsets | θmax = 29.0°, θmin = 2.9° |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | h = −9→10 |
Tmin = 0.924, Tmax = 0.991 | k = −15→15 |
15704 measured reflections | l = −16→18 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0761P)2 + 0.2718P] where P = (Fo2 + 2Fc2)/3 |
5449 reflections | (Δ/σ)max < 0.001 |
354 parameters | Δρmax = 0.35 e Å−3 |
9 restraints | Δρmin = −0.45 e Å−3 |
Crystal data top
C14H22N10Na2O11 | γ = 103.5004 (7)° |
Mr = 552.40 | V = 1074.95 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.5702 (1) Å | Mo Kα radiation |
b = 11.5237 (2) Å | µ = 0.18 mm−1 |
c = 13.3743 (3) Å | T = 150 K |
α = 104.4350 (8)° | 0.45 × 0.25 × 0.05 mm |
β = 97.8415 (8)° | |
Data collection top
Kappa-CCD diffractometer | 5449 independent reflections |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | 4455 reflections with I > 2σ(I) |
Tmin = 0.924, Tmax = 0.991 | Rint = 0.053 |
15704 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.047 | 9 restraints |
wR(F2) = 0.136 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.35 e Å−3 |
5449 reflections | Δρmin = −0.45 e Å−3 |
354 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Na1 | 0.05392 (8) | −0.00233 (5) | 0.63859 (4) | 0.01840 (15) | |
Na2 | 0.44774 (8) | 0.02654 (5) | 0.87001 (4) | 0.01808 (15) | |
N1A | 0.63681 (16) | 0.43063 (11) | 0.62252 (9) | 0.0159 (2) | |
C2A | 0.7496 (2) | 0.35828 (13) | 0.62632 (10) | 0.0153 (3) | |
N2A | 0.68035 (17) | 0.24431 (11) | 0.63286 (10) | 0.0173 (3) | |
C21A | 0.48563 (19) | 0.19257 (13) | 0.62986 (11) | 0.0165 (3) | |
C22A | 0.3659 (2) | 0.12325 (13) | 0.52015 (11) | 0.0157 (3) | |
O21A | 0.20324 (14) | 0.06612 (10) | 0.51894 (8) | 0.0205 (2) | |
O22A | 0.43522 (15) | 0.12875 (11) | 0.44102 (8) | 0.0239 (2) | |
N3A | 0.93659 (17) | 0.39433 (11) | 0.62513 (9) | 0.0163 (2) | |
C3A | 1.0470 (2) | 0.30464 (14) | 0.62079 (13) | 0.0215 (3) | |
C4A | 1.0242 (2) | 0.51581 (13) | 0.62703 (11) | 0.0166 (3) | |
O4A | 1.19040 (15) | 0.54667 (10) | 0.62615 (9) | 0.0236 (2) | |
C5A | 0.9051 (2) | 0.59845 (13) | 0.62927 (10) | 0.0155 (3) | |
N5A | 0.99469 (18) | 0.71658 (11) | 0.64088 (9) | 0.0183 (3) | |
O5A | 0.90055 (15) | 0.79584 (9) | 0.64188 (9) | 0.0219 (2) | |
C6A | 0.7088 (2) | 0.54845 (13) | 0.62214 (10) | 0.0153 (3) | |
N6A | 0.59444 (17) | 0.61854 (11) | 0.61787 (10) | 0.0184 (3) | |
N1B | −0.11087 (16) | −0.40708 (11) | 0.88221 (9) | 0.0161 (2) | |
C2B | −0.22692 (19) | −0.33628 (13) | 0.88301 (10) | 0.0149 (3) | |
N2B | −0.15810 (17) | −0.21679 (11) | 0.88895 (10) | 0.0180 (3) | |
C21B | 0.0372 (2) | −0.16094 (13) | 0.89466 (11) | 0.0177 (3) | |
C22B | 0.14604 (19) | −0.08322 (13) | 1.00496 (11) | 0.0152 (3) | |
O21B | 0.30425 (14) | −0.01441 (10) | 1.00911 (8) | 0.0201 (2) | |
O22B | 0.07505 (15) | −0.09126 (11) | 1.08261 (8) | 0.0258 (3) | |
N3B | −0.41548 (17) | −0.37828 (11) | 0.87654 (9) | 0.0161 (2) | |
C3B | −0.5355 (2) | −0.29641 (14) | 0.86837 (13) | 0.0219 (3) | |
C4B | −0.4978 (2) | −0.50082 (13) | 0.87514 (11) | 0.0163 (3) | |
O4B | −0.66516 (15) | −0.53699 (10) | 0.87057 (9) | 0.0233 (2) | |
C5B | −0.37104 (19) | −0.57757 (13) | 0.88001 (10) | 0.0151 (3) | |
N5B | −0.45236 (17) | −0.69255 (11) | 0.88204 (9) | 0.0175 (3) | |
O5B | −0.35341 (15) | −0.76836 (10) | 0.88634 (9) | 0.0212 (2) | |
C6B | −0.1785 (2) | −0.52597 (13) | 0.88043 (10) | 0.0149 (3) | |
N6B | −0.06301 (17) | −0.59608 (11) | 0.87893 (9) | 0.0177 (3) | |
O1 | 0.21649 (15) | 0.12493 (10) | 0.82016 (8) | 0.0211 (2) | |
O2 | −0.18882 (15) | 0.06565 (9) | 0.70682 (8) | 0.0201 (2) | |
O3 | 0.34158 (17) | −0.11114 (11) | 0.70071 (9) | 0.0318 (3) | |
H2A | 0.7562 | 0.1980 | 0.6393 | 0.021* | |
H21A | 0.4350 | 0.2613 | 0.6626 | 0.020* | |
H21B | 0.4747 | 0.1344 | 0.6736 | 0.020* | |
H3A1 | 1.0636 | 0.2856 | 0.6883 | 0.032* | |
H3A2 | 1.1687 | 0.3407 | 0.6071 | 0.032* | |
H3A3 | 0.9825 | 0.2278 | 0.5641 | 0.032* | |
H6A1 | 0.4756 | 0.5876 | 0.6154 | 0.022* | |
H6A2 | 0.6371 | 0.6963 | 0.6175 | 0.022* | |
H2B | −0.2344 | −0.1696 | 0.8894 | 0.022* | |
H21C | 0.0477 | −0.1072 | 0.8472 | 0.021* | |
H21D | 0.0948 | −0.2282 | 0.8682 | 0.021* | |
H3B1 | −0.5001 | −0.2254 | 0.9324 | 0.033* | |
H3B2 | −0.6652 | −0.3432 | 0.8603 | 0.033* | |
H3B3 | −0.5216 | −0.2659 | 0.8069 | 0.033* | |
H6B1 | 0.0547 | −0.5643 | 0.8791 | 0.021* | |
H6B2 | −0.1037 | −0.6745 | 0.8777 | 0.021* | |
H11 | 0.1242 (18) | 0.1259 (13) | 0.8625 (12) | 0.025* | |
H12 | 0.2985 (18) | 0.2073 (8) | 0.8394 (13) | 0.025* | |
H21 | −0.2809 (19) | −0.0107 (9) | 0.6667 (9) | 0.024* | |
H22 | −0.177 (2) | 0.0690 (13) | 0.7797 (4) | 0.024* | |
H31 | 0.2414 (18) | −0.1862 (11) | 0.6824 (14) | 0.038* | |
H32 | 0.416 (2) | −0.1211 (16) | 0.6480 (12) | 0.038* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0196 (3) | 0.0187 (3) | 0.0180 (3) | 0.0042 (2) | 0.0053 (2) | 0.0076 (2) |
Na2 | 0.0170 (3) | 0.0200 (3) | 0.0180 (3) | 0.0053 (2) | 0.0011 (2) | 0.0079 (2) |
N1A | 0.0143 (6) | 0.0169 (6) | 0.0164 (5) | 0.0049 (4) | 0.0004 (4) | 0.0058 (5) |
C2A | 0.0143 (7) | 0.0188 (7) | 0.0116 (6) | 0.0048 (5) | −0.0012 (5) | 0.0043 (5) |
N2A | 0.0147 (6) | 0.0168 (6) | 0.0201 (6) | 0.0040 (4) | −0.0009 (5) | 0.0075 (5) |
C21A | 0.0141 (7) | 0.0181 (6) | 0.0165 (6) | 0.0028 (5) | 0.0013 (5) | 0.0061 (6) |
C22A | 0.0155 (7) | 0.0168 (6) | 0.0159 (6) | 0.0047 (5) | 0.0026 (5) | 0.0071 (5) |
O21A | 0.0143 (5) | 0.0283 (6) | 0.0166 (5) | 0.0006 (4) | 0.0014 (4) | 0.0087 (4) |
O22A | 0.0181 (5) | 0.0343 (6) | 0.0166 (5) | 0.0021 (4) | 0.0045 (4) | 0.0070 (5) |
N3A | 0.0148 (6) | 0.0168 (6) | 0.0182 (6) | 0.0054 (4) | 0.0025 (5) | 0.0064 (5) |
C3A | 0.0191 (8) | 0.0225 (7) | 0.0274 (8) | 0.0105 (6) | 0.0062 (6) | 0.0101 (6) |
C4A | 0.0146 (7) | 0.0207 (7) | 0.0141 (6) | 0.0040 (5) | 0.0014 (5) | 0.0060 (6) |
O4A | 0.0134 (5) | 0.0253 (6) | 0.0330 (6) | 0.0043 (4) | 0.0058 (4) | 0.0104 (5) |
C5A | 0.0159 (7) | 0.0172 (6) | 0.0139 (6) | 0.0041 (5) | 0.0021 (5) | 0.0068 (5) |
N5A | 0.0189 (6) | 0.0195 (6) | 0.0174 (6) | 0.0052 (5) | 0.0029 (5) | 0.0079 (5) |
O5A | 0.0215 (6) | 0.0182 (5) | 0.0286 (6) | 0.0075 (4) | 0.0026 (4) | 0.0109 (5) |
C6A | 0.0163 (7) | 0.0190 (7) | 0.0106 (6) | 0.0057 (5) | −0.0002 (5) | 0.0053 (5) |
N6A | 0.0148 (6) | 0.0190 (6) | 0.0233 (6) | 0.0059 (5) | 0.0021 (5) | 0.0093 (5) |
N1B | 0.0131 (6) | 0.0175 (6) | 0.0171 (6) | 0.0039 (4) | 0.0007 (4) | 0.0058 (5) |
C2B | 0.0145 (7) | 0.0165 (6) | 0.0118 (6) | 0.0028 (5) | −0.0008 (5) | 0.0042 (5) |
N2B | 0.0152 (6) | 0.0157 (6) | 0.0213 (6) | 0.0033 (4) | −0.0013 (5) | 0.0060 (5) |
C21B | 0.0172 (7) | 0.0175 (7) | 0.0172 (6) | 0.0014 (5) | 0.0023 (5) | 0.0068 (6) |
C22B | 0.0152 (7) | 0.0165 (6) | 0.0161 (6) | 0.0074 (5) | 0.0011 (5) | 0.0067 (5) |
O21B | 0.0149 (5) | 0.0234 (5) | 0.0210 (5) | 0.0026 (4) | −0.0005 (4) | 0.0095 (4) |
O22B | 0.0180 (6) | 0.0440 (7) | 0.0169 (5) | 0.0091 (5) | 0.0042 (4) | 0.0104 (5) |
N3B | 0.0137 (6) | 0.0159 (6) | 0.0184 (6) | 0.0048 (4) | 0.0006 (5) | 0.0053 (5) |
C3B | 0.0178 (7) | 0.0197 (7) | 0.0299 (8) | 0.0085 (6) | 0.0025 (6) | 0.0085 (6) |
C4B | 0.0155 (7) | 0.0176 (7) | 0.0146 (6) | 0.0041 (5) | 0.0013 (5) | 0.0043 (5) |
O4B | 0.0135 (5) | 0.0234 (5) | 0.0329 (6) | 0.0044 (4) | 0.0052 (4) | 0.0088 (5) |
C5B | 0.0150 (7) | 0.0169 (6) | 0.0134 (6) | 0.0040 (5) | 0.0019 (5) | 0.0056 (5) |
N5B | 0.0186 (6) | 0.0175 (6) | 0.0172 (6) | 0.0057 (5) | 0.0030 (5) | 0.0062 (5) |
O5B | 0.0222 (6) | 0.0180 (5) | 0.0264 (5) | 0.0079 (4) | 0.0037 (4) | 0.0101 (4) |
C6B | 0.0159 (7) | 0.0178 (6) | 0.0106 (6) | 0.0048 (5) | 0.0004 (5) | 0.0047 (5) |
N6B | 0.0143 (6) | 0.0180 (6) | 0.0213 (6) | 0.0056 (5) | 0.0017 (5) | 0.0065 (5) |
O1 | 0.0155 (5) | 0.0234 (5) | 0.0240 (5) | 0.0041 (4) | 0.0040 (4) | 0.0073 (5) |
O2 | 0.0213 (6) | 0.0211 (5) | 0.0167 (5) | 0.0069 (4) | −0.0002 (4) | 0.0046 (4) |
O3 | 0.0283 (7) | 0.0304 (6) | 0.0265 (6) | −0.0047 (5) | 0.0133 (5) | −0.0022 (5) |
Geometric parameters (Å, º) top
Na1—O21A | 2.2731 (11) | C6A—N6A | 1.3192 (18) |
Na1—O5Ai | 2.3588 (11) | N6A—H6A1 | 0.8800 |
Na1—O2 | 2.3657 (12) | N6A—H6A2 | 0.8800 |
Na1—O1 | 2.4756 (12) | N1B—C2B | 1.3305 (18) |
Na1—O21Aii | 2.4918 (12) | N1B—C6B | 1.3390 (18) |
Na1—O3 | 2.8819 (15) | C2B—N2B | 1.3316 (18) |
Na1—Na1ii | 3.7020 (11) | C2B—N3B | 1.3792 (18) |
Na1—Na2 | 3.8838 (9) | N2B—C21B | 1.4512 (18) |
Na2—O3 | 2.3253 (13) | N2B—H2B | 0.8800 |
Na2—O21Biii | 2.3591 (12) | C21B—C22B | 1.5239 (19) |
Na2—O21B | 2.3693 (11) | C21B—H21C | 0.9900 |
Na2—O1 | 2.4040 (12) | C21B—H21D | 0.9900 |
Na2—O5Biv | 2.4273 (12) | C22B—O22B | 1.2462 (17) |
Na2—Na2iii | 3.6914 (11) | C22B—O21B | 1.2581 (17) |
N1A—C2A | 1.3299 (18) | C22B—Na2iii | 3.1296 (15) |
N1A—C6A | 1.3413 (18) | O21B—Na2iii | 2.3591 (11) |
C2A—N2A | 1.3249 (18) | N3B—C4B | 1.3984 (18) |
C2A—N3A | 1.3825 (18) | N3B—C3B | 1.4672 (18) |
N2A—C21A | 1.4462 (18) | C3B—H3B1 | 0.9800 |
N2A—H2A | 0.8800 | C3B—H3B2 | 0.9800 |
C21A—C22A | 1.5254 (19) | C3B—H3B3 | 0.9800 |
C21A—H21A | 0.9900 | C4B—O4B | 1.2256 (18) |
C21A—H21B | 0.9900 | C4B—C5B | 1.454 (2) |
C22A—O21A | 1.2495 (17) | C5B—N5B | 1.3330 (18) |
C22A—O22A | 1.2524 (16) | C5B—C6B | 1.4387 (19) |
O21A—Na1ii | 2.4918 (12) | N5B—O5B | 1.2832 (15) |
N3A—C4A | 1.3946 (18) | O5B—Na2i | 2.4273 (12) |
N3A—C3A | 1.4688 (18) | C6B—N6B | 1.3204 (18) |
C3A—H3A1 | 0.9800 | N6B—H6B1 | 0.8800 |
C3A—H3A2 | 0.9800 | N6B—H6B2 | 0.8800 |
C3A—H3A3 | 0.9800 | O1—H11 | 0.958 (15) |
C4A—O4A | 1.2272 (18) | O1—H12 | 0.955 (12) |
C4A—C5A | 1.4543 (19) | O2—H21 | 0.961 (12) |
C5A—N5A | 1.3311 (18) | O2—H22 | 0.957 (6) |
C5A—C6A | 1.4438 (19) | O3—H31 | 0.960 (14) |
N5A—O5A | 1.2817 (15) | O3—H32 | 0.962 (16) |
O5A—Na1iv | 2.3588 (11) | | |
| | | |
O21A—Na1—O5Ai | 131.98 (4) | C6A—N6A—H6A1 | 120.0 |
O21A—Na1—O2 | 126.48 (4) | C6A—N6A—H6A2 | 120.0 |
O5Ai—Na1—O2 | 87.51 (4) | H6A1—N6A—H6A2 | 120.0 |
O21A—Na1—O1 | 110.28 (4) | C2B—N1B—C6B | 118.33 (12) |
O5Ai—Na1—O1 | 108.96 (4) | N1B—C2B—N2B | 118.25 (13) |
O2—Na1—O1 | 78.62 (4) | N1B—C2B—N3B | 124.58 (12) |
O21A—Na1—O21Aii | 78.14 (4) | N2B—C2B—N3B | 117.16 (12) |
O5Ai—Na1—O21Aii | 79.36 (4) | C2B—N2B—C21B | 122.86 (12) |
O2—Na1—O21Aii | 76.14 (4) | C2B—N2B—H2B | 118.6 |
O1—Na1—O21Aii | 153.04 (4) | C21B—N2B—H2B | 118.6 |
O21A—Na1—O3 | 92.13 (4) | N2B—C21B—C22B | 114.43 (11) |
O5Ai—Na1—O3 | 73.93 (4) | N2B—C21B—H21C | 108.7 |
O2—Na1—O3 | 138.44 (4) | C22B—C21B—H21C | 108.7 |
O1—Na1—O3 | 73.15 (4) | N2B—C21B—H21D | 108.7 |
O21Aii—Na1—O3 | 133.29 (4) | C22B—C21B—H21D | 108.7 |
O3—Na2—O21Biii | 122.66 (5) | H21C—C21B—H21D | 107.6 |
O3—Na2—O21B | 119.87 (4) | O22B—C22B—O21B | 125.19 (13) |
O21Biii—Na2—O21B | 77.35 (4) | O22B—C22B—C21B | 119.32 (12) |
O3—Na2—O1 | 85.44 (5) | O21B—C22B—C21B | 115.49 (12) |
O21Biii—Na2—O1 | 151.85 (5) | O22B—C22B—Na2iii | 93.99 (9) |
O21B—Na2—O1 | 90.38 (4) | O21B—C22B—Na2iii | 42.44 (7) |
O3—Na2—O5Biv | 116.79 (4) | C21B—C22B—Na2iii | 135.42 (9) |
O21Biii—Na2—O5Biv | 84.70 (4) | C22B—O21B—Na2iii | 116.47 (9) |
O21B—Na2—O5Biv | 121.43 (4) | C22B—O21B—Na2 | 129.49 (9) |
O1—Na2—O5Biv | 80.27 (4) | Na2iii—O21B—Na2 | 102.65 (4) |
C2A—N1A—C6A | 118.58 (12) | C2B—N3B—C4B | 120.88 (12) |
N2A—C2A—N1A | 118.46 (13) | C2B—N3B—C3B | 120.83 (12) |
N2A—C2A—N3A | 117.17 (12) | C4B—N3B—C3B | 118.27 (12) |
N1A—C2A—N3A | 124.36 (12) | N3B—C3B—H3B1 | 109.5 |
C2A—N2A—C21A | 122.94 (12) | N3B—C3B—H3B2 | 109.5 |
C2A—N2A—H2A | 118.5 | H3B1—C3B—H3B2 | 109.5 |
C21A—N2A—H2A | 118.5 | N3B—C3B—H3B3 | 109.5 |
N2A—C21A—C22A | 115.33 (11) | H3B1—C3B—H3B3 | 109.5 |
N2A—C21A—H21A | 108.4 | H3B2—C3B—H3B3 | 109.5 |
C22A—C21A—H21A | 108.4 | O4B—C4B—N3B | 120.47 (13) |
N2A—C21A—H21B | 108.4 | O4B—C4B—C5B | 124.38 (13) |
C22A—C21A—H21B | 108.4 | N3B—C4B—C5B | 115.14 (12) |
H21A—C21A—H21B | 107.5 | N5B—C5B—C6B | 127.06 (13) |
O21A—C22A—O22A | 126.09 (13) | N5B—C5B—C4B | 113.79 (13) |
O21A—C22A—C21A | 114.96 (11) | C6B—C5B—C4B | 119.14 (12) |
O22A—C22A—C21A | 118.95 (12) | O5B—N5B—C5B | 119.07 (12) |
C22A—O21A—Na1 | 135.07 (9) | N5B—O5B—Na2i | 109.73 (8) |
C22A—O21A—Na1ii | 123.05 (8) | N6B—C6B—N1B | 118.10 (13) |
Na1—O21A—Na1ii | 101.86 (4) | N6B—C6B—C5B | 120.17 (12) |
C2A—N3A—C4A | 121.00 (12) | N1B—C6B—C5B | 121.73 (12) |
C2A—N3A—C3A | 120.49 (12) | C6B—N6B—H6B1 | 120.0 |
C4A—N3A—C3A | 118.51 (12) | C6B—N6B—H6B2 | 120.0 |
N3A—C3A—H3A1 | 109.5 | H6B1—N6B—H6B2 | 120.0 |
N3A—C3A—H3A2 | 109.5 | Na2—O1—Na1 | 105.47 (4) |
H3A1—C3A—H3A2 | 109.5 | Na2—O1—H11 | 114.7 (11) |
N3A—C3A—H3A3 | 109.5 | Na1—O1—H11 | 106.9 (10) |
H3A1—C3A—H3A3 | 109.5 | Na2—O1—H12 | 96.1 (11) |
H3A2—C3A—H3A3 | 109.5 | Na1—O1—H12 | 125.7 (10) |
O4A—C4A—N3A | 120.35 (13) | H11—O1—H12 | 108.0 (7) |
O4A—C4A—C5A | 124.36 (13) | Na1—O2—H21 | 92.8 (10) |
N3A—C4A—C5A | 115.29 (12) | Na1—O2—H22 | 110.4 (10) |
N5A—C5A—C6A | 126.69 (13) | H21—O2—H22 | 107.5 (7) |
N5A—C5A—C4A | 114.23 (13) | Na2—O3—Na1 | 95.87 (4) |
C6A—C5A—C4A | 119.05 (12) | Na2—O3—H31 | 123.9 (10) |
O5A—N5A—C5A | 118.65 (12) | Na1—O3—H31 | 83.9 (12) |
N5A—O5A—Na1iv | 118.26 (9) | Na2—O3—H32 | 124.6 (10) |
N6A—C6A—N1A | 117.65 (13) | Na1—O3—H32 | 110.1 (13) |
N6A—C6A—C5A | 120.91 (13) | H31—O3—H32 | 107.3 (7) |
N1A—C6A—C5A | 121.41 (12) | | |
| | | |
C6A—N1A—C2A—N2A | 176.15 (12) | O3—Na2—O21B—C22B | −20.38 (13) |
C6A—N1A—C2A—N3A | −3.1 (2) | O21Biii—Na2—O21B—C22B | −140.98 (13) |
N1A—C2A—N2A—C21A | 3.7 (2) | O1—Na2—O21B—C22B | 64.58 (12) |
N3A—C2A—N2A—C21A | −177.01 (12) | O5Biv—Na2—O21B—C22B | 143.39 (11) |
C2A—N2A—C21A—C22A | 89.74 (16) | C22Biii—Na2—O21B—C22B | −152.29 (10) |
N2A—C21A—C22A—O21A | 171.76 (12) | Na2iii—Na2—O21B—C22B | −140.98 (13) |
N2A—C21A—C22A—O22A | −8.90 (18) | Na1—Na2—O21B—C22B | 29.97 (12) |
O22A—C22A—O21A—Na1 | 162.20 (11) | O3—Na2—O21B—Na2iii | 120.60 (6) |
C21A—C22A—O21A—Na1 | −18.52 (19) | O21Biii—Na2—O21B—Na2iii | 0.00 (4) |
O22A—C22A—O21A—Na1ii | −19.5 (2) | O1—Na2—O21B—Na2iii | −154.44 (5) |
C21A—C22A—O21A—Na1ii | 159.79 (9) | O5Biv—Na2—O21B—Na2iii | −75.63 (5) |
O5Ai—Na1—O21A—C22A | −117.74 (13) | C22Biii—Na2—O21B—Na2iii | −11.31 (4) |
O2—Na1—O21A—C22A | 115.92 (13) | Na1—Na2—O21B—Na2iii | 170.95 (4) |
O1—Na1—O21A—C22A | 25.25 (14) | N1B—C2B—N3B—C4B | 4.1 (2) |
O21Aii—Na1—O21A—C22A | 178.55 (15) | N2B—C2B—N3B—C4B | −176.91 (12) |
O3—Na1—O21A—C22A | −47.56 (13) | N1B—C2B—N3B—C3B | −174.44 (13) |
Na1ii—Na1—O21A—C22A | 178.55 (15) | N2B—C2B—N3B—C3B | 4.58 (19) |
Na2—Na1—O21A—C22A | −12.82 (14) | C2B—N3B—C4B—O4B | 179.18 (12) |
O5Ai—Na1—O21A—Na1ii | 63.71 (7) | C3B—N3B—C4B—O4B | −2.3 (2) |
O2—Na1—O21A—Na1ii | −62.63 (6) | C2B—N3B—C4B—C5B | −0.50 (19) |
O1—Na1—O21A—Na1ii | −153.30 (5) | C3B—N3B—C4B—C5B | 178.04 (12) |
O21Aii—Na1—O21A—Na1ii | 0.00 (3) | O4B—C4B—C5B—N5B | −1.7 (2) |
O3—Na1—O21A—Na1ii | 133.89 (4) | N3B—C4B—C5B—N5B | 177.92 (11) |
Na2—Na1—O21A—Na1ii | 168.63 (3) | O4B—C4B—C5B—C6B | 177.27 (13) |
N2A—C2A—N3A—C4A | −174.77 (12) | N3B—C4B—C5B—C6B | −3.06 (19) |
N1A—C2A—N3A—C4A | 4.5 (2) | C6B—C5B—N5B—O5B | 1.1 (2) |
N2A—C2A—N3A—C3A | 5.84 (19) | C4B—C5B—N5B—O5B | 180.00 (11) |
N1A—C2A—N3A—C3A | −174.93 (13) | C5B—N5B—O5B—Na2i | −174.01 (10) |
C2A—N3A—C4A—O4A | 179.86 (12) | C2B—N1B—C6B—N6B | 179.55 (12) |
C3A—N3A—C4A—O4A | −0.7 (2) | C2B—N1B—C6B—C5B | −0.4 (2) |
C2A—N3A—C4A—C5A | −0.55 (19) | N5B—C5B—C6B—N6B | 2.6 (2) |
C3A—N3A—C4A—C5A | 178.86 (12) | C4B—C5B—C6B—N6B | −176.25 (12) |
O4A—C4A—C5A—N5A | −6.3 (2) | N5B—C5B—C6B—N1B | −177.46 (13) |
N3A—C4A—C5A—N5A | 174.11 (11) | C4B—C5B—C6B—N1B | 3.7 (2) |
O4A—C4A—C5A—C6A | 175.40 (13) | O3—Na2—O1—Na1 | 2.11 (4) |
N3A—C4A—C5A—C6A | −4.17 (19) | O21Biii—Na2—O1—Na1 | 179.01 (7) |
C6A—C5A—N5A—O5A | −3.1 (2) | O21B—Na2—O1—Na1 | −117.83 (4) |
C4A—C5A—N5A—O5A | 178.80 (11) | O5Biv—Na2—O1—Na1 | 120.30 (4) |
C5A—N5A—O5A—Na1iv | −171.62 (9) | C22Biii—Na2—O1—Na1 | 143.05 (6) |
C2A—N1A—C6A—N6A | 179.71 (12) | Na2iii—Na2—O1—Na1 | −136.91 (4) |
C2A—N1A—C6A—C5A | −2.1 (2) | O21A—Na1—O1—Na2 | −87.73 (5) |
N5A—C5A—C6A—N6A | 5.8 (2) | O5Ai—Na1—O1—Na2 | 64.04 (5) |
C4A—C5A—C6A—N6A | −176.12 (12) | O2—Na1—O1—Na2 | 147.37 (5) |
N5A—C5A—C6A—N1A | −172.33 (13) | O21Aii—Na1—O1—Na2 | 168.21 (7) |
C4A—C5A—C6A—N1A | 5.7 (2) | O3—Na1—O1—Na2 | −1.77 (4) |
C6B—N1B—C2B—N2B | 177.41 (12) | Na1ii—Na1—O1—Na2 | −118.26 (6) |
C6B—N1B—C2B—N3B | −3.6 (2) | O21Biii—Na2—O3—Na1 | 179.98 (4) |
N1B—C2B—N2B—C21B | −0.1 (2) | O21B—Na2—O3—Na1 | 86.06 (5) |
N3B—C2B—N2B—C21B | −179.15 (12) | O1—Na2—O3—Na1 | −1.75 (4) |
C2B—N2B—C21B—C22B | −101.62 (15) | O5Biv—Na2—O3—Na1 | −78.44 (5) |
N2B—C21B—C22B—O22B | 13.31 (18) | C22Biii—Na2—O3—Na1 | −154.99 (4) |
N2B—C21B—C22B—O21B | −166.48 (11) | Na2iii—Na2—O3—Na1 | 131.98 (5) |
N2B—C21B—C22B—Na2iii | 146.45 (10) | O21A—Na1—O3—Na2 | 112.33 (4) |
O22B—C22B—O21B—Na2iii | 49.83 (17) | O5Ai—Na1—O3—Na2 | −114.37 (5) |
C21B—C22B—O21B—Na2iii | −130.40 (10) | O2—Na1—O3—Na2 | −47.51 (8) |
O22B—C22B—O21B—Na2 | −173.51 (10) | O1—Na1—O3—Na2 | 1.77 (4) |
C21B—C22B—O21B—Na2 | 6.27 (17) | O21Aii—Na1—O3—Na2 | −172.01 (4) |
Na2iii—C22B—O21B—Na2 | 136.66 (14) | Na1ii—Na1—O3—Na2 | 145.19 (4) |
Symmetry codes: (i) x−1, y−1, z; (ii) −x, −y, −z+1; (iii) −x+1, −y, −z+2; (iv) x+1, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2A—H2A···O2v | 0.88 | 2.05 | 2.810 (2) | 144 |
N2B—H2B···O21Bvi | 0.88 | 2.43 | 3.187 (2) | 144 |
N6A—H6A1···O4Avii | 0.88 | 2.13 | 3.002 (2) | 169 |
N6A—H62A···O5A | 0.88 | 1.99 | 2.628 (2) | 128 |
N6B—H6B1···O4Bv | 0.88 | 2.09 | 2.953 (2) | 165 |
N6B—H6B2···O5B | 0.88 | 1.98 | 2.628 (2) | 129 |
O1—H11···O22Bvi | 0.96 (2) | 1.77 (2) | 2.711 (2) | 166 (1) |
O1—H12···N5Biv | 0.96 (1) | 1.89 (1) | 2.738 (2) | 146 (1) |
O2—H21···O22Aii | 0.96 (1) | 1.76 (1) | 2.691 (2) | 161 (1) |
O2—H22···O22Bvi | 0.96 (1) | 1.83 (1) | 2.751 (2) | 161 (1) |
O3—H31···N5Ai | 0.96 (1) | 1.87 (1) | 2.771 (2) | 156 (1) |
O3—H32···O22Aviii | 0.96 (2) | 1.75 (2) | 2.708 (2) | 175 (1) |
Symmetry codes: (i) x−1, y−1, z; (ii) −x, −y, −z+1; (iv) x+1, y+1, z; (v) x+1, y, z; (vi) −x, −y, −z+2; (vii) x−1, y, z; (viii) −x+1, −y, −z+1. |
(3) Aqua-
N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-
oxopyrimidin-2-yl)glycinatopotassium
top
Crystal data top
C7H10KN5O5 | F(000) = 584 |
Mr = 283.30 | Dx = 1.737 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 7.8114 (2) Å | Cell parameters from 2814 reflections |
b = 16.4811 (5) Å | θ = 2.9–29.0° |
c = 8.5560 (2) Å | µ = 0.52 mm−1 |
β = 100.408 (2)° | T = 150 K |
V = 1083.38 (5) Å3 | Block, red |
Z = 4 | 0.10 × 0.10 × 0.05 mm |
Data collection top
Kappa-CCD diffractometer | 2814 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 2226 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
ϕ scans and ω scans with κ offsets | θmax = 29.0°, θmin = 2.9° |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | h = −10→10 |
Tmin = 0.950, Tmax = 0.975 | k = −19→23 |
8482 measured reflections | l = −11→11 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.052P)2 + 0.1977P] where P = (Fo2 + 2Fc2)/3 |
2814 reflections | (Δ/σ)max = 0.001 |
170 parameters | Δρmax = 0.34 e Å−3 |
3 restraints | Δρmin = −0.50 e Å−3 |
Crystal data top
C7H10KN5O5 | V = 1083.38 (5) Å3 |
Mr = 283.30 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.8114 (2) Å | µ = 0.52 mm−1 |
b = 16.4811 (5) Å | T = 150 K |
c = 8.5560 (2) Å | 0.10 × 0.10 × 0.05 mm |
β = 100.408 (2)° | |
Data collection top
Kappa-CCD diffractometer | 2814 independent reflections |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | 2226 reflections with I > 2σ(I) |
Tmin = 0.950, Tmax = 0.975 | Rint = 0.046 |
8482 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.042 | 3 restraints |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.34 e Å−3 |
2814 reflections | Δρmin = −0.50 e Å−3 |
170 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.46135 (5) | 0.25777 (2) | 0.69176 (4) | 0.01931 (14) | |
N1 | 0.17520 (19) | 0.40422 (9) | 0.56971 (16) | 0.0171 (3) | |
C2 | 0.1470 (2) | 0.42211 (10) | 0.41549 (19) | 0.0143 (3) | |
N2 | 0.05109 (18) | 0.37122 (9) | 0.31546 (16) | 0.0164 (3) | |
C21 | −0.0327 (2) | 0.30124 (10) | 0.3721 (2) | 0.0169 (4) | |
C22 | 0.0856 (2) | 0.22960 (10) | 0.42938 (19) | 0.0151 (3) | |
O21 | 0.23875 (16) | 0.22893 (8) | 0.40508 (14) | 0.0194 (3) | |
O22 | 0.01458 (16) | 0.17404 (7) | 0.49617 (14) | 0.0206 (3) | |
C3 | 0.1604 (3) | 0.50720 (11) | 0.1815 (2) | 0.0220 (4) | |
N3 | 0.20734 (18) | 0.49089 (8) | 0.35225 (15) | 0.0152 (3) | |
C4 | 0.3059 (2) | 0.54870 (10) | 0.4488 (2) | 0.0172 (4) | |
O4 | 0.35827 (17) | 0.60912 (7) | 0.38895 (15) | 0.0247 (3) | |
C5 | 0.3391 (2) | 0.53054 (10) | 0.6177 (2) | 0.0165 (4) | |
N5 | 0.4309 (2) | 0.58701 (9) | 0.70871 (17) | 0.0212 (3) | |
O5 | 0.47143 (17) | 0.57318 (8) | 0.85983 (14) | 0.0254 (3) | |
C6 | 0.2719 (2) | 0.45560 (10) | 0.67092 (19) | 0.0155 (3) | |
N6 | 0.3054 (2) | 0.43546 (9) | 0.82198 (17) | 0.0203 (3) | |
O1 | 0.66183 (17) | 0.30429 (8) | 0.97742 (14) | 0.0223 (3) | |
H2 | 0.0380 | 0.3801 | 0.2126 | 0.020* | |
H21A | −0.1252 | 0.2822 | 0.2852 | 0.020* | |
H21B | −0.0898 | 0.3190 | 0.4606 | 0.020* | |
H3A | 0.1998 | 0.4622 | 0.1220 | 0.033* | |
H3B | 0.2162 | 0.5576 | 0.1563 | 0.033* | |
H3C | 0.0338 | 0.5127 | 0.1519 | 0.033* | |
H6A | 0.2647 | 0.3897 | 0.8536 | 0.024* | |
H6B | 0.3684 | 0.4678 | 0.8915 | 0.024* | |
H11 | 0.7840 (8) | 0.3119 (10) | 0.980 (2) | 0.027* | |
H12 | 0.6177 (19) | 0.3529 (7) | 1.017 (2) | 0.027* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0193 (2) | 0.0210 (2) | 0.0180 (2) | −0.00012 (14) | 0.00447 (16) | −0.00195 (14) |
N1 | 0.0203 (8) | 0.0161 (7) | 0.0149 (7) | −0.0019 (6) | 0.0033 (6) | −0.0007 (6) |
C2 | 0.0156 (9) | 0.0111 (8) | 0.0171 (8) | 0.0025 (6) | 0.0052 (7) | 0.0008 (6) |
N2 | 0.0191 (8) | 0.0154 (7) | 0.0140 (7) | −0.0023 (6) | 0.0010 (6) | 0.0016 (5) |
C21 | 0.0144 (8) | 0.0146 (8) | 0.0210 (8) | −0.0021 (6) | 0.0013 (7) | 0.0012 (7) |
C22 | 0.0169 (9) | 0.0150 (8) | 0.0121 (7) | −0.0019 (7) | −0.0008 (6) | −0.0035 (6) |
O21 | 0.0167 (6) | 0.0213 (7) | 0.0208 (6) | 0.0005 (5) | 0.0045 (5) | −0.0029 (5) |
O22 | 0.0214 (7) | 0.0186 (7) | 0.0219 (6) | −0.0010 (5) | 0.0038 (5) | 0.0055 (5) |
C3 | 0.0297 (11) | 0.0193 (9) | 0.0169 (8) | −0.0024 (8) | 0.0037 (7) | 0.0026 (7) |
N3 | 0.0186 (8) | 0.0122 (7) | 0.0152 (7) | −0.0007 (6) | 0.0041 (6) | 0.0004 (5) |
C4 | 0.0166 (9) | 0.0134 (8) | 0.0225 (9) | 0.0008 (7) | 0.0064 (7) | −0.0013 (7) |
O4 | 0.0312 (8) | 0.0164 (7) | 0.0273 (7) | −0.0072 (5) | 0.0078 (6) | 0.0017 (5) |
C5 | 0.0162 (9) | 0.0127 (8) | 0.0210 (8) | 0.0013 (6) | 0.0043 (7) | −0.0015 (7) |
N5 | 0.0207 (8) | 0.0181 (8) | 0.0239 (8) | 0.0022 (6) | 0.0009 (6) | −0.0030 (6) |
O5 | 0.0280 (8) | 0.0223 (7) | 0.0228 (7) | 0.0019 (6) | −0.0034 (6) | −0.0055 (5) |
C6 | 0.0141 (8) | 0.0151 (8) | 0.0179 (8) | 0.0022 (6) | 0.0049 (6) | −0.0014 (7) |
N6 | 0.0249 (8) | 0.0190 (8) | 0.0164 (7) | −0.0036 (6) | 0.0021 (6) | −0.0006 (6) |
O1 | 0.0215 (7) | 0.0217 (7) | 0.0247 (7) | 0.0001 (5) | 0.0066 (5) | −0.0016 (5) |
Geometric parameters (Å, º) top
K1—O21i | 2.7476 (12) | C3—N3 | 1.466 (2) |
K1—O4ii | 2.7616 (13) | C3—H3A | 0.9800 |
K1—O1 | 2.7624 (13) | C3—H3B | 0.9800 |
K1—O21 | 2.7794 (12) | C3—H3C | 0.9800 |
K1—O1iii | 2.8106 (13) | N3—C4 | 1.398 (2) |
K1—N5iv | 3.0157 (15) | C4—O4 | 1.223 (2) |
K1—O5iv | 3.1320 (13) | C4—C5 | 1.453 (2) |
N1—C2 | 1.331 (2) | O4—K1ii | 2.7616 (13) |
N1—C6 | 1.342 (2) | C5—N5 | 1.336 (2) |
C2—N2 | 1.329 (2) | C5—C6 | 1.447 (2) |
C2—N3 | 1.375 (2) | N5—O5 | 1.2946 (19) |
N2—C21 | 1.452 (2) | N5—K1v | 3.0157 (15) |
N2—H2 | 0.8800 | O5—K1v | 3.1320 (13) |
C21—C22 | 1.524 (2) | C6—N6 | 1.314 (2) |
C21—H21A | 0.9900 | N6—H6A | 0.8800 |
C21—H21B | 0.9900 | N6—H6B | 0.8800 |
C22—O21 | 1.251 (2) | O1—K1i | 2.8106 (13) |
C22—O22 | 1.260 (2) | O1—H11 | 0.959 (7) |
O21—K1iii | 2.7476 (12) | O1—H12 | 0.958 (13) |
| | | |
O21i—K1—O4ii | 121.03 (4) | C22—K1—K1iii | 59.13 (3) |
O21i—K1—O1 | 73.49 (4) | N6—K1—K1iii | 116.03 (3) |
O4ii—K1—O1 | 76.55 (4) | K1i—K1—K1iii | 173.15 (2) |
O21i—K1—O21 | 103.28 (4) | C2—N1—C6 | 118.23 (14) |
O4ii—K1—O21 | 100.44 (4) | C2—N1—K1 | 116.96 (10) |
O1—K1—O21 | 173.01 (4) | C6—N1—K1 | 89.27 (10) |
O21i—K1—O1iii | 163.04 (4) | N2—C2—N1 | 118.15 (15) |
O4ii—K1—O1iii | 75.90 (4) | N2—C2—N3 | 117.40 (14) |
O1—K1—O1iii | 112.63 (5) | N1—C2—N3 | 124.44 (15) |
O21—K1—O1iii | 72.27 (4) | C2—N2—C21 | 121.47 (13) |
O21i—K1—N5iv | 93.71 (4) | C2—N2—H2 | 119.3 |
O4ii—K1—N5iv | 133.08 (4) | C21—N2—H2 | 119.3 |
O1—K1—N5iv | 85.67 (4) | N2—C21—C22 | 116.06 (14) |
O21—K1—N5iv | 100.82 (4) | N2—C21—H21A | 108.3 |
O1iii—K1—N5iv | 71.62 (4) | C22—C21—H21A | 108.3 |
O21i—K1—O5iv | 108.26 (4) | N2—C21—H21B | 108.3 |
O4ii—K1—O5iv | 129.07 (4) | C22—C21—H21B | 108.3 |
O1—K1—O5iv | 108.16 (4) | H21A—C21—H21B | 107.4 |
O21—K1—O5iv | 78.67 (4) | O21—C22—O22 | 125.57 (16) |
O1iii—K1—O5iv | 55.05 (4) | O21—C22—C21 | 119.71 (15) |
N5iv—K1—O5iv | 24.22 (4) | O22—C22—C21 | 114.70 (15) |
O21i—K1—N1 | 71.38 (4) | O21—C22—K1 | 51.06 (8) |
O4ii—K1—N1 | 71.90 (4) | O22—C22—K1 | 101.46 (10) |
O1—K1—N1 | 108.52 (4) | C21—C22—K1 | 120.58 (10) |
O21—K1—N1 | 64.49 (4) | C22—O21—K1iii | 148.09 (11) |
O1iii—K1—N1 | 118.76 (4) | C22—O21—K1 | 108.45 (10) |
N5iv—K1—N1 | 154.56 (4) | K1iii—O21—K1 | 101.68 (4) |
O5iv—K1—N1 | 141.32 (4) | N3—C3—H3A | 109.5 |
O21i—K1—C22 | 82.80 (4) | N3—C3—H3B | 109.5 |
O4ii—K1—C22 | 111.29 (4) | H3A—C3—H3B | 109.5 |
O1—K1—C22 | 155.32 (4) | N3—C3—H3C | 109.5 |
O21—K1—C22 | 20.49 (4) | H3A—C3—H3C | 109.5 |
O1iii—K1—C22 | 92.06 (4) | H3B—C3—H3C | 109.5 |
N5iv—K1—C22 | 102.90 (4) | C2—N3—C4 | 121.38 (13) |
O5iv—K1—C22 | 85.46 (4) | C2—N3—C3 | 120.11 (14) |
N1—K1—C22 | 55.89 (4) | C4—N3—C3 | 118.42 (14) |
O21i—K1—N6 | 54.00 (4) | O4—C4—N3 | 119.85 (15) |
O4ii—K1—N6 | 68.32 (4) | O4—C4—C5 | 124.83 (16) |
O1—K1—N6 | 69.75 (4) | N3—C4—C5 | 115.32 (14) |
O21—K1—N6 | 103.30 (4) | C4—O4—K1ii | 167.28 (12) |
O1iii—K1—N6 | 142.58 (4) | N5—C5—C6 | 126.76 (15) |
N5iv—K1—N6 | 143.27 (4) | N5—C5—C4 | 114.61 (15) |
O5iv—K1—N6 | 162.25 (4) | C6—C5—C4 | 118.63 (15) |
N1—K1—N6 | 39.24 (3) | O5—N5—C5 | 117.89 (15) |
C22—K1—N6 | 90.92 (4) | O5—N5—K1v | 82.93 (9) |
O21i—K1—K1i | 39.43 (3) | C5—N5—K1v | 155.18 (12) |
O4ii—K1—K1i | 112.90 (3) | N5—O5—K1v | 72.85 (9) |
O1—K1—K1i | 40.15 (3) | N6—C6—N1 | 117.65 (16) |
O21—K1—K1i | 139.28 (3) | N6—C6—C5 | 120.39 (15) |
O1iii—K1—K1i | 136.89 (3) | N1—C6—C5 | 121.96 (15) |
N5iv—K1—K1i | 73.30 (3) | C6—N6—K1 | 85.15 (10) |
O5iv—K1—K1i | 96.48 (3) | C6—N6—H6A | 120.0 |
N1—K1—K1i | 103.62 (3) | K1—N6—H6A | 62.4 |
C22—K1—K1i | 119.79 (3) | C6—N6—H6B | 120.0 |
N6—K1—K1i | 70.31 (3) | K1—N6—H6B | 123.2 |
O21i—K1—K1iii | 141.44 (3) | H6A—N6—H6B | 120.0 |
O4ii—K1—K1iii | 72.89 (3) | K1—O1—K1i | 100.53 (4) |
O1—K1—K1iii | 142.90 (3) | K1—O1—H11 | 117.5 (11) |
O21—K1—K1iii | 38.89 (3) | K1i—O1—H11 | 134.4 (12) |
O1iii—K1—K1iii | 39.33 (3) | K1—O1—H12 | 111.2 (11) |
N5iv—K1—K1iii | 100.12 (3) | K1i—O1—H12 | 78.2 (11) |
O5iv—K1—K1iii | 76.76 (2) | H11—O1—H12 | 107.5 (7) |
N1—K1—K1iii | 81.44 (2) | | |
| | | |
O21i—K1—N1—C2 | −156.46 (12) | C21—C22—O21—K1 | 106.98 (14) |
O4ii—K1—N1—C2 | 70.52 (12) | O21i—K1—O21—C22 | 1.44 (10) |
O1—K1—N1—C2 | 138.96 (11) | O4ii—K1—O21—C22 | −124.15 (11) |
O21—K1—N1—C2 | −41.03 (11) | O1iii—K1—O21—C22 | 164.45 (12) |
O1iii—K1—N1—C2 | 8.66 (13) | N5iv—K1—O21—C22 | 97.91 (11) |
N5iv—K1—N1—C2 | −99.78 (14) | O5iv—K1—O21—C22 | 107.77 (11) |
O5iv—K1—N1—C2 | −60.24 (13) | N1—K1—O21—C22 | −60.13 (11) |
C22—K1—N1—C2 | −62.53 (11) | N6—K1—O21—C22 | −54.17 (11) |
N6—K1—N1—C2 | 148.15 (14) | K1i—K1—O21—C22 | 20.99 (13) |
K1i—K1—N1—C2 | −179.48 (11) | K1iii—K1—O21—C22 | −169.33 (13) |
K1iii—K1—N1—C2 | −4.19 (11) | O21i—K1—O21—K1iii | 170.77 (5) |
O21i—K1—N1—C6 | 81.93 (10) | O4ii—K1—O21—K1iii | 45.18 (5) |
O4ii—K1—N1—C6 | −51.09 (9) | O1iii—K1—O21—K1iii | −26.22 (4) |
O1—K1—N1—C6 | 17.35 (10) | N5iv—K1—O21—K1iii | −92.75 (4) |
O21—K1—N1—C6 | −162.64 (10) | O5iv—K1—O21—K1iii | −82.90 (4) |
O1iii—K1—N1—C6 | −112.95 (10) | N1—K1—O21—K1iii | 109.21 (5) |
N5iv—K1—N1—C6 | 138.61 (11) | C22—K1—O21—K1iii | 169.33 (13) |
O5iv—K1—N1—C6 | 178.15 (9) | N6—K1—O21—K1iii | 115.16 (4) |
C22—K1—N1—C6 | 175.85 (11) | K1i—K1—O21—K1iii | −169.67 (3) |
N6—K1—N1—C6 | 26.54 (9) | N2—C2—N3—C4 | 178.58 (15) |
K1i—K1—N1—C6 | 58.90 (9) | N1—C2—N3—C4 | 0.1 (2) |
K1iii—K1—N1—C6 | −125.80 (9) | N2—C2—N3—C3 | 2.1 (2) |
C6—N1—C2—N2 | −179.94 (15) | N1—C2—N3—C3 | −176.42 (16) |
K1—N1—C2—N2 | 75.19 (17) | C2—N3—C4—O4 | 179.74 (15) |
C6—N1—C2—N3 | −1.4 (2) | C3—N3—C4—O4 | −3.7 (2) |
K1—N1—C2—N3 | −106.31 (15) | C2—N3—C4—C5 | 0.1 (2) |
N1—C2—N2—C21 | 4.8 (2) | C3—N3—C4—C5 | 176.64 (14) |
N3—C2—N2—C21 | −173.85 (14) | N3—C4—O4—K1ii | −146.9 (4) |
C2—N2—C21—C22 | −76.0 (2) | C5—C4—O4—K1ii | 32.8 (6) |
N2—C21—C22—O21 | −10.0 (2) | O4—C4—C5—N5 | 1.4 (3) |
N2—C21—C22—O22 | 171.48 (14) | N3—C4—C5—N5 | −178.92 (15) |
N2—C21—C22—K1 | 49.76 (18) | O4—C4—C5—C6 | −178.60 (16) |
O21i—K1—C22—O21 | −178.59 (10) | N3—C4—C5—C6 | 1.0 (2) |
O4ii—K1—C22—O21 | 60.86 (12) | C6—C5—N5—O5 | 2.9 (3) |
O1—K1—C22—O21 | 165.35 (11) | C4—C5—N5—O5 | −177.18 (14) |
O1iii—K1—C22—O21 | −14.80 (11) | C6—C5—N5—K1v | −141.5 (2) |
N5iv—K1—C22—O21 | −86.42 (11) | C4—C5—N5—K1v | 38.5 (3) |
O5iv—K1—C22—O21 | −69.50 (11) | C5—N5—O5—K1v | −165.73 (15) |
N1—K1—C22—O21 | 109.06 (12) | C2—N1—C6—N6 | −177.01 (15) |
N6—K1—C22—O21 | 127.89 (11) | K1—N1—C6—N6 | −56.49 (14) |
K1i—K1—C22—O21 | −164.38 (10) | C2—N1—C6—C5 | 2.6 (2) |
K1iii—K1—C22—O21 | 7.78 (10) | K1—N1—C6—C5 | 123.12 (15) |
O21i—K1—C22—O22 | −51.77 (10) | N5—C5—C6—N6 | −2.9 (3) |
O4ii—K1—C22—O22 | −172.32 (10) | C4—C5—C6—N6 | 177.14 (15) |
O1—K1—C22—O22 | −67.83 (15) | N5—C5—C6—N1 | 177.47 (16) |
O21—K1—C22—O22 | 126.82 (17) | C4—C5—C6—N1 | −2.5 (2) |
O1iii—K1—C22—O22 | 112.02 (10) | N1—C6—N6—K1 | 54.16 (14) |
N5iv—K1—C22—O22 | 40.41 (11) | C5—C6—N6—K1 | −125.46 (14) |
O5iv—K1—C22—O22 | 57.32 (10) | O21i—K1—N6—C6 | −132.66 (11) |
N1—K1—C22—O22 | −124.12 (12) | O4ii—K1—N6—C6 | 60.35 (10) |
N6—K1—C22—O22 | −105.29 (10) | O1—K1—N6—C6 | 143.45 (11) |
K1i—K1—C22—O22 | −37.56 (11) | O21—K1—N6—C6 | −35.76 (10) |
K1iii—K1—C22—O22 | 134.60 (11) | O1iii—K1—N6—C6 | 42.35 (13) |
O21i—K1—C22—C21 | 76.19 (12) | N5iv—K1—N6—C6 | −165.51 (9) |
O4ii—K1—C22—C21 | −44.36 (13) | O5iv—K1—N6—C6 | −130.15 (13) |
O1—K1—C22—C21 | 60.13 (17) | N1—K1—N6—C6 | −27.25 (9) |
O21—K1—C22—C21 | −105.22 (17) | C22—K1—N6—C6 | −52.25 (10) |
O1iii—K1—C22—C21 | −120.02 (12) | K1i—K1—N6—C6 | −173.71 (10) |
N5iv—K1—C22—C21 | 168.36 (12) | K1iii—K1—N6—C6 | 3.47 (11) |
O5iv—K1—C22—C21 | −174.73 (12) | O21i—K1—O1—K1i | 26.09 (4) |
N1—K1—C22—C21 | 3.84 (11) | O4ii—K1—O1—K1i | 154.68 (5) |
N6—K1—C22—C21 | 22.67 (12) | O1iii—K1—O1—K1i | −137.10 (5) |
K1i—K1—C22—C21 | 90.40 (12) | N5iv—K1—O1—K1i | −69.07 (4) |
K1iii—K1—C22—C21 | −97.44 (12) | O5iv—K1—O1—K1i | −78.20 (5) |
O22—C22—O21—K1iii | 125.35 (19) | N1—K1—O1—K1i | 89.32 (4) |
C21—C22—O21—K1iii | −53.0 (3) | C22—K1—O1—K1i | 42.73 (11) |
K1—C22—O21—K1iii | −159.9 (2) | N6—K1—O1—K1i | 83.13 (4) |
O22—C22—O21—K1 | −74.70 (18) | K1iii—K1—O1—K1i | −170.15 (3) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z−1/2; (iv) −x+1, y−1/2, −z+3/2; (v) −x+1, y+1/2, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O22iii | 0.88 | 2.03 | 2.796 (2) | 144 |
N6—H6A···O21i | 0.88 | 2.02 | 2.872 (2) | 162 |
N6—H6B···O5 | 0.88 | 1.95 | 2.605 (2) | 130 |
O1—H11···O22vi | 0.96 (1) | 1.80 (1) | 2.754 (2) | 177 (2) |
O1—H12···O5vii | 0.96 (1) | 1.83 (1) | 2.761 (2) | 164 (1) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (iii) x, −y+1/2, z−1/2; (vi) x+1, −y+1/2, z+1/2; (vii) −x+1, −y+1, −z+2. |
(MnL2) Tetraaqua-bis[
N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-
oxopyrimidin-2-yl)glycinato]manganese(II) hexahydrate
top
Crystal data top
C14H24MnN10O12·6(H2O) | Z = 1 |
Mr = 687.46 | F(000) = 359 |
Triclinic, P1 | Dx = 1.629 Mg m−3 |
a = 7.4476 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.2351 (4) Å | Cell parameters from 3131 reflections |
c = 12.6372 (5) Å | θ = 1.7–27.5° |
α = 105.258 (2)° | µ = 0.57 mm−1 |
β = 92.153 (3)° | T = 150 K |
γ = 108.94 (2)° | Plate, red |
V = 700.81 (5) Å3 | 0.45 × 0.35 × 0.08 mm |
Data collection top
Kappa-CCD diffractometer | 3131 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 2814 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.068 |
ϕ scans and ω scans with κ offsets | θmax = 27.5°, θmin = 1.7° |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | h = −9→9 |
Tmin = 0.784, Tmax = 0.959 | k = −10→10 |
7489 measured reflections | l = −15→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0452P)2 + 0.4451P] where P = (Fo2 + 2Fc2)/3 |
3131 reflections | (Δ/σ)max = 0.006 |
233 parameters | Δρmax = 0.50 e Å−3 |
15 restraints | Δρmin = −0.57 e Å−3 |
Crystal data top
C14H24MnN10O12·6(H2O) | γ = 108.94 (2)° |
Mr = 687.46 | V = 700.81 (5) Å3 |
Triclinic, P1 | Z = 1 |
a = 7.4476 (3) Å | Mo Kα radiation |
b = 8.2351 (4) Å | µ = 0.57 mm−1 |
c = 12.6372 (5) Å | T = 150 K |
α = 105.258 (2)° | 0.45 × 0.35 × 0.08 mm |
β = 92.153 (3)° | |
Data collection top
Kappa-CCD diffractometer | 3131 independent reflections |
Absorption correction: multi-scan SORTAV (Blessing, 1995 & 1997) | 2814 reflections with I > 2σ(I) |
Tmin = 0.784, Tmax = 0.959 | Rint = 0.068 |
7489 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.040 | 15 restraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.10 | Δρmax = 0.50 e Å−3 |
3131 reflections | Δρmin = −0.57 e Å−3 |
233 parameters | |
Special details top
Geometry. Mean-plane data from the final SHELXL97 refinement run:- |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 0.5000 | 0.0000 | 0.5000 | 0.01698 (13) | |
N1 | 0.1453 (2) | 0.1486 (2) | 0.91956 (13) | 0.0187 (3) | |
C2 | −0.0347 (3) | 0.0625 (2) | 0.87141 (15) | 0.0173 (4) | |
N2 | −0.0704 (2) | −0.0790 (2) | 0.78329 (13) | 0.0197 (3) | |
C21 | 0.0819 (3) | −0.1344 (3) | 0.73489 (16) | 0.0206 (4) | |
C22 | 0.1847 (2) | −0.0280 (2) | 0.65941 (14) | 0.0171 (4) | |
O21 | 0.32251 (18) | −0.07366 (18) | 0.62267 (11) | 0.0211 (3) | |
O22 | 0.13010 (19) | 0.08985 (18) | 0.63825 (11) | 0.0219 (3) | |
C3 | −0.3836 (3) | 0.0089 (3) | 0.84736 (17) | 0.0247 (4) | |
N3 | −0.1892 (2) | 0.1080 (2) | 0.90783 (13) | 0.0184 (3) | |
C4 | −0.1650 (3) | 0.2478 (3) | 1.00356 (15) | 0.0187 (4) | |
O4 | −0.3040 (2) | 0.2836 (2) | 1.03735 (12) | 0.0269 (3) | |
C5 | 0.0298 (3) | 0.3443 (3) | 1.05824 (15) | 0.0179 (4) | |
N5 | 0.0466 (2) | 0.4789 (2) | 1.14923 (13) | 0.0217 (3) | |
O5 | 0.2152 (2) | 0.5711 (2) | 1.20237 (12) | 0.0270 (3) | |
C6 | 0.1810 (3) | 0.2877 (3) | 1.01120 (15) | 0.0178 (4) | |
N6 | 0.3591 (2) | 0.3701 (2) | 1.05951 (14) | 0.0226 (3) | |
O1W | 0.4172 (2) | 0.23277 (18) | 0.52434 (12) | 0.0241 (3) | |
O2W | 0.2367 (2) | −0.1481 (2) | 0.37756 (12) | 0.0276 (3) | |
O3W | 0.3797 (2) | 0.36643 (19) | 0.35193 (13) | 0.0294 (3) | |
O4W | 0.1927 (3) | 0.5302 (3) | 0.5202 (2) | 0.0554 (6) | |
O5W | 0.6924 (3) | 0.5341 (2) | 0.25271 (16) | 0.0458 (5) | |
H2 | −0.1899 | −0.1411 | 0.7533 | 0.024* | |
H21A | 0.0271 | −0.2627 | 0.6919 | 0.025* | |
H21B | 0.1774 | −0.1232 | 0.7955 | 0.025* | |
H3A | −0.3815 | 0.0022 | 0.7689 | 0.037* | |
H3B | −0.4704 | 0.0712 | 0.8779 | 0.037* | |
H3C | −0.4282 | −0.1127 | 0.8551 | 0.037* | |
H6A | 0.4508 | 0.3338 | 1.0317 | 0.027* | |
H6B | 0.3867 | 0.4617 | 1.1197 | 0.027* | |
H1W1 | 0.2982 (17) | 0.206 (3) | 0.5541 (16) | 0.029* | |
H2W1 | 0.402 (3) | 0.275 (3) | 0.4621 (13) | 0.029* | |
H1W2 | 0.121 (2) | −0.121 (3) | 0.377 (2) | 0.043 (7)* | |
H2W2 | 0.210 (4) | −0.266 (2) | 0.328 (2) | 0.084 (12)* | |
H1W3 | 0.494 (3) | 0.434 (3) | 0.329 (3) | 0.087 (12)* | |
H2W3 | 0.323 (4) | 0.449 (3) | 0.392 (3) | 0.077 (11)* | |
H1W4 | 0.067 (3) | 0.511 (5) | 0.488 (4) | 0.135 (19)* | |
H2W4 | 0.258 (5) | 0.6570 (12) | 0.550 (3) | 0.104 (15)* | |
H1W5 | 0.762 (3) | 0.480 (3) | 0.2016 (19) | 0.055* | |
H2W5 | 0.769 (3) | 0.6574 (13) | 0.286 (2) | 0.055* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0180 (2) | 0.0183 (2) | 0.0164 (2) | 0.00734 (15) | 0.00728 (14) | 0.00576 (15) |
N1 | 0.0156 (7) | 0.0238 (8) | 0.0203 (8) | 0.0099 (6) | 0.0075 (6) | 0.0079 (6) |
C2 | 0.0173 (8) | 0.0234 (9) | 0.0178 (8) | 0.0099 (7) | 0.0087 (7) | 0.0122 (7) |
N2 | 0.0163 (7) | 0.0247 (8) | 0.0194 (8) | 0.0074 (6) | 0.0081 (6) | 0.0077 (7) |
C21 | 0.0210 (9) | 0.0234 (9) | 0.0212 (9) | 0.0104 (7) | 0.0105 (7) | 0.0083 (7) |
C22 | 0.0151 (8) | 0.0195 (9) | 0.0137 (8) | 0.0038 (7) | 0.0028 (6) | 0.0026 (7) |
O21 | 0.0198 (6) | 0.0285 (7) | 0.0204 (7) | 0.0115 (5) | 0.0098 (5) | 0.0108 (6) |
O22 | 0.0223 (7) | 0.0236 (7) | 0.0244 (7) | 0.0103 (5) | 0.0090 (5) | 0.0106 (6) |
C3 | 0.0155 (9) | 0.0340 (11) | 0.0248 (10) | 0.0097 (8) | 0.0044 (7) | 0.0075 (8) |
N3 | 0.0145 (7) | 0.0254 (8) | 0.0189 (8) | 0.0091 (6) | 0.0067 (6) | 0.0088 (6) |
C4 | 0.0197 (9) | 0.0265 (9) | 0.0179 (9) | 0.0137 (7) | 0.0084 (7) | 0.0117 (8) |
O4 | 0.0200 (7) | 0.0376 (8) | 0.0275 (7) | 0.0169 (6) | 0.0095 (6) | 0.0069 (6) |
C5 | 0.0189 (9) | 0.0240 (9) | 0.0174 (8) | 0.0118 (7) | 0.0073 (7) | 0.0106 (7) |
N5 | 0.0236 (8) | 0.0266 (8) | 0.0199 (8) | 0.0130 (7) | 0.0055 (6) | 0.0092 (7) |
O5 | 0.0240 (7) | 0.0308 (8) | 0.0236 (7) | 0.0108 (6) | 0.0021 (6) | 0.0019 (6) |
C6 | 0.0175 (8) | 0.0242 (9) | 0.0180 (8) | 0.0103 (7) | 0.0071 (7) | 0.0119 (7) |
N6 | 0.0159 (7) | 0.0290 (9) | 0.0237 (8) | 0.0111 (6) | 0.0047 (6) | 0.0047 (7) |
O1W | 0.0269 (7) | 0.0226 (7) | 0.0280 (7) | 0.0124 (6) | 0.0112 (6) | 0.0100 (6) |
O2W | 0.0214 (7) | 0.0315 (8) | 0.0244 (7) | 0.0103 (6) | −0.0007 (6) | −0.0020 (6) |
O3W | 0.0343 (8) | 0.0224 (7) | 0.0306 (8) | 0.0082 (6) | 0.0051 (6) | 0.0079 (6) |
O4W | 0.0279 (9) | 0.0410 (11) | 0.1016 (18) | 0.0133 (8) | 0.0171 (10) | 0.0247 (11) |
O5W | 0.0495 (10) | 0.0259 (8) | 0.0551 (11) | 0.0082 (7) | 0.0353 (9) | 0.0028 (8) |
Geometric parameters (Å, º) top
Mn1—O1W | 2.1498 (13) | C3—H3C | 0.9800 |
Mn1—O1Wi | 2.1498 (13) | N3—C4 | 1.392 (2) |
Mn1—O21i | 2.1555 (12) | C4—O4 | 1.227 (2) |
Mn1—O21 | 2.1556 (12) | C4—C5 | 1.449 (3) |
Mn1—O2W | 2.2254 (14) | C5—N5 | 1.340 (3) |
Mn1—O2Wi | 2.2254 (15) | C5—C6 | 1.444 (2) |
N1—C2 | 1.328 (2) | N5—O5 | 1.286 (2) |
N1—C6 | 1.344 (2) | C6—N6 | 1.315 (2) |
C2—N2 | 1.327 (3) | N6—H6A | 0.8800 |
C2—N3 | 1.381 (2) | N6—H6B | 0.8800 |
N2—C21 | 1.452 (2) | O1W—H1W1 | 0.96 (2) |
N2—H2 | 0.8800 | O1W—H2W1 | 0.96 (2) |
C21—C22 | 1.524 (2) | O2W—H1W2 | 0.96 (2) |
C21—H21A | 0.9900 | O2W—H2W2 | 0.96 (2) |
C21—H21B | 0.9900 | O3W—H1W3 | 0.96 (3) |
C22—O22 | 1.250 (2) | O3W—H2W3 | 0.96 (3) |
C22—O21 | 1.267 (2) | O4W—H1W4 | 0.95 (3) |
C3—N3 | 1.472 (2) | O4W—H2W4 | 0.96 (2) |
C3—H3A | 0.9800 | O5W—H1W5 | 0.95 (2) |
C3—H3B | 0.9800 | O5W—H2W5 | 0.96 (2) |
| | | |
O1W—Mn1—O1Wi | 180.0 | N3—C3—H3A | 109.5 |
O1W—Mn1—O21i | 91.84 (5) | N3—C3—H3B | 109.5 |
O1Wi—Mn1—O21i | 88.16 (5) | H3A—C3—H3B | 109.5 |
O1W—Mn1—O21 | 88.16 (5) | N3—C3—H3C | 109.5 |
O1Wi—Mn1—O21 | 91.84 (5) | H3A—C3—H3C | 109.5 |
O21i—Mn1—O21 | 180.0 | H3B—C3—H3C | 109.5 |
O1W—Mn1—O2W | 87.15 (6) | C2—N3—C4 | 120.64 (16) |
O1Wi—Mn1—O2W | 92.85 (6) | C2—N3—C3 | 120.96 (16) |
O21i—Mn1—O2W | 93.72 (5) | C4—N3—C3 | 118.39 (15) |
O21—Mn1—O2W | 86.28 (5) | O4—C4—N3 | 120.23 (17) |
O1W—Mn1—O2Wi | 92.85 (6) | O4—C4—C5 | 123.57 (17) |
O1Wi—Mn1—O2Wi | 87.15 (6) | N3—C4—C5 | 116.20 (15) |
O21i—Mn1—O2Wi | 86.28 (5) | N5—C5—C6 | 127.45 (17) |
O21—Mn1—O2Wi | 93.72 (5) | N5—C5—C4 | 114.18 (15) |
O2W—Mn1—O2Wi | 180.0 | C6—C5—C4 | 118.37 (16) |
C2—N1—C6 | 118.46 (15) | O5—N5—C5 | 117.91 (15) |
N2—C2—N1 | 118.28 (16) | N6—C6—N1 | 118.07 (16) |
N2—C2—N3 | 117.25 (16) | N6—C6—C5 | 120.10 (17) |
N1—C2—N3 | 124.45 (17) | N1—C6—C5 | 121.81 (17) |
C2—N2—C21 | 121.97 (16) | C6—N6—H6A | 120.0 |
C2—N2—H2 | 119.0 | C6—N6—H6B | 120.0 |
C21—N2—H2 | 119.0 | H6A—N6—H6B | 120.0 |
N2—C21—C22 | 114.76 (15) | Mn1—O1W—H1W1 | 106.8 (13) |
N2—C21—H21A | 108.6 | Mn1—O1W—H2W1 | 118.6 (14) |
C22—C21—H21A | 108.6 | H1W1—O1W—H2W1 | 108 (2) |
N2—C21—H21B | 108.6 | Mn1—O2W—H1W2 | 126.6 (14) |
C22—C21—H21B | 108.6 | Mn1—O2W—H2W2 | 124.1 (15) |
H21A—C21—H21B | 107.6 | H1W2—O2W—H2W2 | 108 (2) |
O22—C22—O21 | 126.21 (16) | H1W3—O3W—H2W3 | 108 (2) |
O22—C22—C21 | 120.52 (15) | H1W4—O4W—H2W4 | 108 (3) |
O21—C22—C21 | 113.27 (16) | H1W5—O5W—H2W5 | 109 (2) |
C22—O21—Mn1 | 131.54 (12) | | |
| | | |
C6—N1—C2—N2 | −177.54 (16) | C2—N3—C4—O4 | −177.60 (16) |
C6—N1—C2—N3 | 1.3 (3) | C3—N3—C4—O4 | 1.7 (3) |
N1—C2—N2—C21 | −3.8 (3) | C2—N3—C4—C5 | 2.4 (2) |
N3—C2—N2—C21 | 177.24 (15) | C3—N3—C4—C5 | −178.33 (16) |
C2—N2—C21—C22 | −80.4 (2) | O4—C4—C5—N5 | −0.7 (3) |
N2—C21—C22—O22 | −3.8 (3) | N3—C4—C5—N5 | 179.25 (15) |
N2—C21—C22—O21 | 176.85 (15) | O4—C4—C5—C6 | 179.13 (17) |
O22—C22—O21—Mn1 | −7.5 (3) | N3—C4—C5—C6 | −0.9 (2) |
C21—C22—O21—Mn1 | 171.83 (12) | C6—C5—N5—O5 | 0.2 (3) |
O1W—Mn1—O21—C22 | 20.30 (16) | C4—C5—N5—O5 | −179.93 (15) |
O1Wi—Mn1—O21—C22 | −159.70 (16) | C2—N1—C6—N6 | 178.78 (16) |
O2W—Mn1—O21—C22 | −66.96 (16) | C2—N1—C6—C5 | 0.3 (3) |
O2Wi—Mn1—O21—C22 | 113.04 (16) | N5—C5—C6—N6 | 0.9 (3) |
N2—C2—N3—C4 | 176.06 (15) | C4—C5—C6—N6 | −178.90 (16) |
N1—C2—N3—C4 | −2.8 (3) | N5—C5—C6—N1 | 179.34 (17) |
N2—C2—N3—C3 | −3.2 (2) | C4—C5—C6—N1 | −0.5 (3) |
N1—C2—N3—C3 | 177.98 (17) | | |
Symmetry code: (i) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O3Wii | 0.88 | 2.02 | 2.804 (2) | 148 |
N6—H6A···O4iii | 0.88 | 2.00 | 2.828 (2) | 156 |
N6—H6B···O5 | 0.88 | 1.97 | 2.620 (2) | 130 |
O1W—H1W1···O22 | 0.96 (2) | 1.86 (2) | 2.742 (2) | 151 (2) |
O1W—H2W1···O3W | 0.96 (2) | 1.77 (2) | 2.731 (2) | 177 (2) |
O2W—H1W2···O22ii | 0.96 (2) | 1.98 (2) | 2.933 (2) | 174 (2) |
O2W—H2W2···O5iv | 0.96 (2) | 1.80 (2) | 2.705 (2) | 156 (2) |
O3W—H1W3···O5W | 0.96 (3) | 1.88 (3) | 2.817 (3) | 167 (3) |
O3W—H2W3···O4W | 0.96 (3) | 2.00 (3) | 2.865 (3) | 150 (3) |
O4W—H1W4···O4Wv | 0.95 (3) | 1.85 (3) | 2.754 (3) | 158 (4) |
O4W—H2W4···O21vi | 0.96 (2) | 2.05 (2) | 2.981 (3) | 164 (3) |
O5W—H1W5···O4vii | 0.95 (2) | 2.19 (2) | 2.958 (2) | 137 (2) |
O5W—H1W5···N5vii | 0.95 (2) | 2.24 (2) | 3.100 (3) | 148 (2) |
O5W—H2W5···O22viii | 0.96 (2) | 1.92 (2) | 2.864 (2) | 167 (2) |
Symmetry codes: (ii) −x, −y, −z+1; (iii) x+1, y, z; (iv) x, y−1, z−1; (v) −x, −y+1, −z+1; (vi) x, y+1, z; (vii) x+1, y, z−1; (viii) −x+1, −y+1, −z+1. |
Experimental details
| (1) | (190) | (3) | (MnL2) |
Crystal data |
Chemical formula | C7H14LiN5O7 | C14H22N10Na2O11 | C7H10KN5O5 | C14H24MnN10O12·6(H2O) |
Mr | 287.17 | 552.40 | 283.30 | 687.46 |
Crystal system, space group | Monoclinic, C2/c | Triclinic, P1 | Monoclinic, P21/c | Triclinic, P1 |
Temperature (K) | 150 | 150 | 150 | 150 |
a, b, c (Å) | 24.7736 (6), 7.6525 (3), 14.0096 (5) | 7.5702 (1), 11.5237 (2), 13.3743 (3) | 7.8114 (2), 16.4811 (5), 8.5560 (2) | 7.4476 (3), 8.2351 (4), 12.6372 (5) |
α, β, γ (°) | 90, 114.3751 (13), 90 | 104.4350 (8), 97.8415 (8), 103.5004 (7) | 90, 100.408 (2), 90 | 105.258 (2), 92.153 (3), 108.94 (2) |
V (Å3) | 2419.20 (14) | 1074.95 (3) | 1083.38 (5) | 700.81 (5) |
Z | 8 | 2 | 4 | 1 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.14 | 0.18 | 0.52 | 0.57 |
Crystal size (mm) | 0.20 × 0.10 × 0.10 | 0.45 × 0.25 × 0.05 | 0.10 × 0.10 × 0.05 | 0.45 × 0.35 × 0.08 |
|
Data collection |
Diffractometer | Kappa-CCD diffractometer | Kappa-CCD diffractometer | Kappa-CCD diffractometer | Kappa-CCD diffractometer |
Absorption correction | Multi-scan SORTAV (Blessing, 1995 & 1997) | Multi-scan SORTAV (Blessing, 1995 & 1997) | Multi-scan SORTAV (Blessing, 1995 & 1997) | Multi-scan SORTAV (Blessing, 1995 & 1997) |
Tmin, Tmax | 0.973, 0.986 | 0.924, 0.991 | 0.950, 0.975 | 0.784, 0.959 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7232, 2637, 2024 | 15704, 5449, 4455 | 8482, 2814, 2226 | 7489, 3131, 2814 |
Rint | 0.027 | 0.053 | 0.046 | 0.068 |
(sin θ/λ)max (Å−1) | 0.649 | 0.682 | 0.682 | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.121, 1.03 | 0.047, 0.136, 1.04 | 0.042, 0.108, 1.07 | 0.040, 0.107, 1.10 |
No. of reflections | 2637 | 5449 | 2814 | 3131 |
No. of parameters | 200 | 354 | 170 | 233 |
No. of restraints | 9 | 9 | 3 | 15 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.24, −0.30 | 0.35, −0.45 | 0.34, −0.50 | 0.50, −0.57 |
Hydrogen-bond geometry (Å, º) for (MnL2) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O3Wi | 0.88 | 2.02 | 2.804 (2) | 148 |
N6—H6A···O4ii | 0.88 | 2.00 | 2.828 (2) | 156 |
N6—H6B···O5 | 0.88 | 1.97 | 2.620 (2) | 130 |
O1W—H1W1···O22 | 0.96 (2) | 1.86 (2) | 2.742 (2) | 151 (2) |
O1W—H2W1···O3W | 0.96 (2) | 1.77 (2) | 2.731 (2) | 177 (2) |
O2W—H1W2···O22i | 0.96 (2) | 1.98 (2) | 2.933 (2) | 174 (2) |
O2W—H2W2···O5iii | 0.96 (2) | 1.80 (2) | 2.705 (2) | 156 (2) |
O3W—H1W3···O5W | 0.96 (3) | 1.88 (3) | 2.817 (3) | 167 (3) |
O3W—H2W3···O4W | 0.96 (3) | 2.00 (3) | 2.865 (3) | 150 (3) |
O4W—H1W4···O4Wiv | 0.95 (3) | 1.85 (3) | 2.754 (3) | 158 (4) |
O4W—H2W4···O21v | 0.96 (2) | 2.05 (2) | 2.981 (3) | 164 (3) |
O5W—H1W5···O4vi | 0.95 (2) | 2.19 (2) | 2.958 (2) | 137 (2) |
O5W—H1W5···N5vi | 0.95 (2) | 2.24 (2) | 3.100 (3) | 148 (2) |
O5W—H2W5···O22vii | 0.96 (2) | 1.92 (2) | 2.864 (2) | 167 (2) |
Symmetry codes: (i) −x, −y, −z+1; (ii) x+1, y, z; (iii) x, y−1, z−1; (iv) −x, −y+1, −z+1; (v) x, y+1, z; (vi) x+1, y, z−1; (vii) −x+1, −y+1, −z+1. |
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