Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100020280/na0116sup1.cif
Contains datablocks global, 1, 190, 3, MnL2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100020280/na01161sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100020280/na01162sup3.hkl
Contains datablock 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100020280/na01163sup4.hkl
Contains datablock 3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100020280/na01164sup5.hkl
Contains datablock 4

CCDC references: 166498; 166499; 166500; 166501

Comment top

In full text version

Experimental top

In full text version

Refinement top

In full text version

Computing details top

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
[Figure 11]
[Figure 12]
[Figure 13]
[Figure 14]
[Figure 15]
[Figure 16]
[Figure 17]
[Figure 18]
In full text version
(1) Triaqua-N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidine-2-yl) glycinatolithium, top
Crystal data top
C7H14LiN5O7F(000) = 1200
Mr = 287.17Dx = 1.577 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 24.7736 (6) ÅCell parameters from 2637 reflections
b = 7.6525 (3) Åθ = 3.0–27.5°
c = 14.0096 (5) ŵ = 0.14 mm1
β = 114.3751 (13)°T = 150 K
V = 2419.20 (14) Å3Block, red
Z = 80.20 × 0.10 × 0.10 mm
Data collection top
Kappa-CCD
diffractometer
2637 independent reflections
Radiation source: fine-focus sealed X-ray tube2024 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ϕ scans and ω scans with κ offsetsθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
SORTAV (Blessing, 1995 & 1997)
h = 3232
Tmin = 0.973, Tmax = 0.986k = 99
7232 measured reflectionsl = 1818
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.121H-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 parametersΔρmax = 0.24 e Å3
9 restraintsΔρmin = 0.30 e Å3
Crystal data top
C7H14LiN5O7V = 2419.20 (14) Å3
Mr = 287.17Z = 8
Monoclinic, C2/cMo Kα radiation
a = 24.7736 (6) ŵ = 0.14 mm1
b = 7.6525 (3) ÅT = 150 K
c = 14.0096 (5) Å0.20 × 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 = 0.986Rint = 0.027
7232 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0459 restraints
wR(F2) = 0.121H-atom parameters constrained
S = 1.03Δρmax = 0.24 e Å3
2637 reflectionsΔρmin = 0.30 e Å3
200 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Li10.29248 (13)0.3873 (4)0.1674 (2)0.0209 (6)
N10.44897 (6)0.77584 (19)0.11599 (12)0.0173 (3)
C20.42022 (7)0.9234 (2)0.11378 (13)0.0160 (4)
N20.36671 (6)0.91241 (19)0.11396 (11)0.0182 (3)
H20.34561.00810.10600.022*
C210.34233 (7)0.7469 (2)0.12697 (14)0.0187 (4)
H21A0.31210.77020.15460.022*
H21B0.37440.67830.18060.022*
C220.31410 (7)0.6355 (2)0.02917 (13)0.0152 (4)
O210.29906 (5)0.48528 (15)0.04541 (9)0.0188 (3)
O220.30629 (5)0.69571 (15)0.05865 (9)0.0202 (3)
N30.44254 (6)1.08863 (18)0.11320 (11)0.0165 (3)
C30.40555 (8)1.2438 (2)0.10341 (15)0.0230 (4)
H3A0.36701.22820.04430.034*
H3B0.42521.34720.09140.034*
H3C0.39981.25920.16810.034*
C40.50067 (7)1.1121 (2)0.12467 (13)0.0160 (4)
O40.52105 (5)1.25971 (15)0.13151 (10)0.0221 (3)
C50.53312 (7)0.9528 (2)0.12704 (13)0.0164 (4)
N50.58835 (6)0.98110 (19)0.13560 (11)0.0183 (3)
O50.61943 (5)0.84596 (16)0.13552 (10)0.0213 (3)
C60.50410 (7)0.7866 (2)0.12094 (13)0.0167 (4)
N60.53190 (6)0.63922 (19)0.12209 (11)0.0198 (3)
H6A0.51420.53850.11960.024*
H6B0.56810.64150.12530.024*
O10.35831 (5)0.39663 (16)0.30945 (9)0.0207 (3)
H110.3391 (7)0.383 (2)0.3560 (11)0.025*
H120.3898 (6)0.3123 (19)0.3294 (13)0.025*
O20.27923 (5)0.13984 (16)0.14011 (9)0.0198 (3)
H210.2744 (7)0.089 (2)0.1984 (7)0.024*
H220.2485 (6)0.096 (2)0.0771 (6)0.024*
O30.22339 (5)0.50360 (16)0.17302 (9)0.0198 (3)
H310.2134 (6)0.6065 (14)0.1305 (12)0.024*
H320.1875 (4)0.4410 (18)0.1594 (14)0.024*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Li10.0203 (14)0.0192 (15)0.0242 (16)0.0007 (12)0.0103 (13)0.0009 (13)
N10.0143 (7)0.0166 (7)0.0201 (8)0.0010 (6)0.0061 (6)0.0003 (6)
C20.0161 (8)0.0177 (8)0.0125 (9)0.0030 (7)0.0042 (7)0.0020 (7)
N20.0154 (7)0.0176 (7)0.0211 (8)0.0013 (6)0.0072 (6)0.0018 (6)
C210.0180 (8)0.0192 (9)0.0189 (10)0.0032 (7)0.0077 (7)0.0018 (7)
C220.0112 (7)0.0166 (8)0.0188 (9)0.0023 (7)0.0074 (7)0.0003 (7)
O210.0225 (6)0.0153 (6)0.0185 (7)0.0018 (5)0.0085 (5)0.0006 (5)
O220.0243 (6)0.0200 (6)0.0171 (7)0.0009 (5)0.0094 (5)0.0025 (5)
N30.0158 (7)0.0145 (7)0.0185 (8)0.0007 (6)0.0063 (6)0.0006 (6)
C30.0229 (9)0.0158 (9)0.0312 (11)0.0013 (7)0.0120 (8)0.0004 (8)
C40.0173 (8)0.0183 (9)0.0122 (9)0.0018 (7)0.0058 (7)0.0011 (7)
O40.0223 (7)0.0155 (6)0.0289 (8)0.0032 (5)0.0109 (6)0.0004 (5)
C50.0169 (8)0.0169 (8)0.0144 (9)0.0009 (7)0.0055 (7)0.0002 (7)
N50.0161 (7)0.0209 (7)0.0171 (8)0.0006 (6)0.0062 (6)0.0019 (6)
O50.0172 (6)0.0215 (6)0.0253 (7)0.0043 (5)0.0089 (5)0.0024 (5)
C60.0174 (8)0.0183 (9)0.0122 (9)0.0001 (7)0.0039 (7)0.0003 (7)
N60.0166 (7)0.0147 (7)0.0278 (9)0.0002 (6)0.0087 (7)0.0003 (6)
O10.0182 (6)0.0239 (7)0.0204 (7)0.0014 (5)0.0083 (5)0.0017 (5)
O20.0211 (6)0.0187 (6)0.0181 (7)0.0028 (5)0.0067 (5)0.0010 (5)
O30.0181 (6)0.0187 (6)0.0232 (7)0.0009 (5)0.0092 (5)0.0031 (5)
Geometric parameters (Å, º) top
Li1—O21.933 (3)C3—H3A0.9800
Li1—O211.934 (3)C3—H3B0.9800
Li1—O31.959 (3)C3—H3C0.9800
Li1—O11.986 (3)C4—O41.2248 (19)
N1—C21.329 (2)C4—C51.453 (2)
N1—C61.341 (2)C5—N51.341 (2)
C2—N21.329 (2)C5—C61.446 (2)
C2—N31.381 (2)N5—O51.2896 (19)
N2—C211.447 (2)C6—N61.318 (2)
N2—H20.8800N6—H6A0.8800
C21—C221.517 (2)N6—H6B0.8800
C21—H21A0.9900O1—H110.959 (17)
C21—H21B0.9900O1—H120.961 (16)
C22—O221.252 (2)O2—H210.956 (13)
C22—O211.258 (2)O2—H220.957 (10)
N3—C41.393 (2)O3—H310.956 (12)
N3—C31.471 (2)O3—H320.957 (13)
O2—Li1—O21105.91 (15)N3—C3—H3B109.5
O2—Li1—O3111.91 (14)H3A—C3—H3B109.5
O21—Li1—O3104.65 (14)N3—C3—H3C109.5
O2—Li1—O1103.63 (14)H3A—C3—H3C109.5
O21—Li1—O1122.51 (15)H3B—C3—H3C109.5
O3—Li1—O1108.26 (15)O4—C4—N3120.07 (15)
C2—N1—C6118.28 (14)O4—C4—C5124.45 (15)
N1—C2—N2118.14 (15)N3—C4—C5115.48 (14)
N1—C2—N3124.48 (15)N5—C5—C6127.70 (15)
N2—C2—N3117.38 (15)N5—C5—C4113.63 (14)
C2—N2—C21121.62 (14)C6—C5—C4118.67 (15)
C2—N2—H2119.2O5—N5—C5117.25 (14)
C21—N2—H2119.2N6—C6—N1117.64 (15)
N2—C21—C22116.04 (14)N6—C6—C5120.49 (15)
N2—C21—H21A108.3N1—C6—C5121.86 (15)
C22—C21—H21A108.3C6—N6—H6A120.0
N2—C21—H21B108.3C6—N6—H6B120.0
C22—C21—H21B108.3H6A—N6—H6B120.0
H21A—C21—H21B107.4Li1—O1—H11104.1 (11)
O22—C22—O21125.25 (15)Li1—O1—H12120.0 (11)
O22—C22—C21120.47 (15)H11—O1—H12107.5 (7)
O21—C22—C21114.26 (14)Li1—O2—H21107.5 (10)
C22—O21—Li1130.81 (14)Li1—O2—H22122.0 (11)
C2—N3—C4120.97 (14)H21—O2—H22108.2 (7)
C2—N3—C3120.25 (13)Li1—O3—H31110.8 (10)
C4—N3—C3118.76 (13)Li1—O3—H32121.3 (11)
N3—C3—H3A109.5H31—O3—H32107.9 (7)
C6—N1—C2—N2176.83 (15)C2—N3—C4—O4174.77 (15)
C6—N1—C2—N31.9 (3)C3—N3—C4—O43.5 (2)
N1—C2—N2—C216.2 (2)C2—N3—C4—C55.5 (2)
N3—C2—N2—C21172.61 (15)C3—N3—C4—C5176.18 (14)
C2—N2—C21—C2281.9 (2)O4—C4—C5—N51.2 (3)
N2—C21—C22—O228.6 (2)N3—C4—C5—N5178.47 (14)
N2—C21—C22—O21172.84 (14)O4—C4—C5—C6178.40 (16)
O22—C22—O21—Li1165.69 (16)N3—C4—C5—C61.9 (2)
C21—C22—O21—Li112.8 (2)C6—C5—N5—O52.2 (3)
O2—Li1—O21—C22171.10 (14)C4—C5—N5—O5178.28 (14)
O3—Li1—O21—C2270.5 (2)C2—N1—C6—N6179.38 (15)
O1—Li1—O21—C2252.9 (3)C2—N1—C6—C51.9 (3)
N1—C2—N3—C46.0 (3)N5—C5—C6—N61.0 (3)
N2—C2—N3—C4172.82 (15)C4—C5—C6—N6179.51 (15)
N1—C2—N3—C3175.80 (16)N5—C5—C6—N1177.74 (16)
N2—C2—N3—C35.4 (2)C4—C5—C6—N11.8 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O2i0.882.142.918 (2)146
N6—H6A···O4ii0.882.142.925 (2)148
N6—H6B···O1iii0.882.513.100 (2)125
O1—H11···O22iv0.96 (2)1.80 (2)2.746 (2)167 (1)
O1—H12···O4v0.96 (2)2.08 (2)2.945 (2)148 (1)
O2—H21···O3vi0.96 (1)1.90 (1)2.844 (2)171 (1)
O2—H22···O21vii0.96 (1)1.75 (1)2.697 (2)171 (1)
O3—H31···O22viii0.96 (1)1.77 (1)2.726 (2)176 (1)
O3—H32···O5ix0.96 (1)1.74 (1)2.692 (2)175 (1)
Symmetry codes: (i) x, y+1, z; (ii) x, y1, z; (iii) x+1, y, z+1/2; (iv) x, y+1, z+1/2; (v) x+1, y1, z+1/2; (vi) x+1/2, y1/2, z+1/2; (vii) x+1/2, y+1/2, z; (viii) x+1/2, y+3/2, z; (ix) x1/2, y1/2, z.
(190) Triaqua-bis[N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4- oxopyrimidin-2-yl)glycinato]disodium top
Crystal data top
C14H22N10Na2O11Z = 2
Mr = 552.40F(000) = 572
Triclinic, P1Dx = 1.707 Mg m3
a = 7.5702 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.5237 (2) ÅCell parameters from 5449 reflections
c = 13.3743 (3) Åθ = 2.9–29.0°
α = 104.4350 (8)°µ = 0.18 mm1
β = 97.8415 (8)°T = 150 K
γ = 103.5004 (7)°Plate, colourless
V = 1074.95 (3) Å30.45 × 0.25 × 0.05 mm
Data collection top
Kappa-CCD
diffractometer
5449 independent reflections
Radiation source: fine-focus sealed X-ray tube4455 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.053
ϕ scans and ω scans with κ offsetsθmax = 29.0°, θmin = 2.9°
Absorption correction: multi-scan
SORTAV (Blessing, 1995 & 1997)
h = 910
Tmin = 0.924, Tmax = 0.991k = 1515
15704 measured reflectionsl = 1618
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.136H-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 parametersΔρmax = 0.35 e Å3
9 restraintsΔρmin = 0.45 e Å3
Crystal data top
C14H22N10Na2O11γ = 103.5004 (7)°
Mr = 552.40V = 1074.95 (3) Å3
Triclinic, P1Z = 2
a = 7.5702 (1) ÅMo Kα radiation
b = 11.5237 (2) ŵ = 0.18 mm1
c = 13.3743 (3) ÅT = 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 = 0.991Rint = 0.053
15704 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0479 restraints
wR(F2) = 0.136H-atom parameters constrained
S = 1.04Δρmax = 0.35 e Å3
5449 reflectionsΔρmin = 0.45 e Å3
354 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Na10.05392 (8)0.00233 (5)0.63859 (4)0.01840 (15)
Na20.44774 (8)0.02654 (5)0.87001 (4)0.01808 (15)
N1A0.63681 (16)0.43063 (11)0.62252 (9)0.0159 (2)
C2A0.7496 (2)0.35828 (13)0.62632 (10)0.0153 (3)
N2A0.68035 (17)0.24431 (11)0.63286 (10)0.0173 (3)
C21A0.48563 (19)0.19257 (13)0.62986 (11)0.0165 (3)
C22A0.3659 (2)0.12325 (13)0.52015 (11)0.0157 (3)
O21A0.20324 (14)0.06612 (10)0.51894 (8)0.0205 (2)
O22A0.43522 (15)0.12875 (11)0.44102 (8)0.0239 (2)
N3A0.93659 (17)0.39433 (11)0.62513 (9)0.0163 (2)
C3A1.0470 (2)0.30464 (14)0.62079 (13)0.0215 (3)
C4A1.0242 (2)0.51581 (13)0.62703 (11)0.0166 (3)
O4A1.19040 (15)0.54667 (10)0.62615 (9)0.0236 (2)
C5A0.9051 (2)0.59845 (13)0.62927 (10)0.0155 (3)
N5A0.99469 (18)0.71658 (11)0.64088 (9)0.0183 (3)
O5A0.90055 (15)0.79584 (9)0.64188 (9)0.0219 (2)
C6A0.7088 (2)0.54845 (13)0.62214 (10)0.0153 (3)
N6A0.59444 (17)0.61854 (11)0.61787 (10)0.0184 (3)
N1B0.11087 (16)0.40708 (11)0.88221 (9)0.0161 (2)
C2B0.22692 (19)0.33628 (13)0.88301 (10)0.0149 (3)
N2B0.15810 (17)0.21679 (11)0.88895 (10)0.0180 (3)
C21B0.0372 (2)0.16094 (13)0.89466 (11)0.0177 (3)
C22B0.14604 (19)0.08322 (13)1.00496 (11)0.0152 (3)
O21B0.30425 (14)0.01441 (10)1.00911 (8)0.0201 (2)
O22B0.07505 (15)0.09126 (11)1.08261 (8)0.0258 (3)
N3B0.41548 (17)0.37828 (11)0.87654 (9)0.0161 (2)
C3B0.5355 (2)0.29641 (14)0.86837 (13)0.0219 (3)
C4B0.4978 (2)0.50082 (13)0.87514 (11)0.0163 (3)
O4B0.66516 (15)0.53699 (10)0.87057 (9)0.0233 (2)
C5B0.37104 (19)0.57757 (13)0.88001 (10)0.0151 (3)
N5B0.45236 (17)0.69255 (11)0.88204 (9)0.0175 (3)
O5B0.35341 (15)0.76836 (10)0.88634 (9)0.0212 (2)
C6B0.1785 (2)0.52597 (13)0.88043 (10)0.0149 (3)
N6B0.06301 (17)0.59608 (11)0.87893 (9)0.0177 (3)
O10.21649 (15)0.12493 (10)0.82016 (8)0.0211 (2)
O20.18882 (15)0.06565 (9)0.70682 (8)0.0201 (2)
O30.34158 (17)0.11114 (11)0.70071 (9)0.0318 (3)
H2A0.75620.19800.63930.021*
H21A0.43500.26130.66260.020*
H21B0.47470.13440.67360.020*
H3A11.06360.28560.68830.032*
H3A21.16870.34070.60710.032*
H3A30.98250.22780.56410.032*
H6A10.47560.58760.61540.022*
H6A20.63710.69630.61750.022*
H2B0.23440.16960.88940.022*
H21C0.04770.10720.84720.021*
H21D0.09480.22820.86820.021*
H3B10.50010.22540.93240.033*
H3B20.66520.34320.86030.033*
H3B30.52160.26590.80690.033*
H6B10.05470.56430.87910.021*
H6B20.10370.67450.87770.021*
H110.1242 (18)0.1259 (13)0.8625 (12)0.025*
H120.2985 (18)0.2073 (8)0.8394 (13)0.025*
H210.2809 (19)0.0107 (9)0.6667 (9)0.024*
H220.177 (2)0.0690 (13)0.7797 (4)0.024*
H310.2414 (18)0.1862 (11)0.6824 (14)0.038*
H320.416 (2)0.1211 (16)0.6480 (12)0.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0196 (3)0.0187 (3)0.0180 (3)0.0042 (2)0.0053 (2)0.0076 (2)
Na20.0170 (3)0.0200 (3)0.0180 (3)0.0053 (2)0.0011 (2)0.0079 (2)
N1A0.0143 (6)0.0169 (6)0.0164 (5)0.0049 (4)0.0004 (4)0.0058 (5)
C2A0.0143 (7)0.0188 (7)0.0116 (6)0.0048 (5)0.0012 (5)0.0043 (5)
N2A0.0147 (6)0.0168 (6)0.0201 (6)0.0040 (4)0.0009 (5)0.0075 (5)
C21A0.0141 (7)0.0181 (6)0.0165 (6)0.0028 (5)0.0013 (5)0.0061 (6)
C22A0.0155 (7)0.0168 (6)0.0159 (6)0.0047 (5)0.0026 (5)0.0071 (5)
O21A0.0143 (5)0.0283 (6)0.0166 (5)0.0006 (4)0.0014 (4)0.0087 (4)
O22A0.0181 (5)0.0343 (6)0.0166 (5)0.0021 (4)0.0045 (4)0.0070 (5)
N3A0.0148 (6)0.0168 (6)0.0182 (6)0.0054 (4)0.0025 (5)0.0064 (5)
C3A0.0191 (8)0.0225 (7)0.0274 (8)0.0105 (6)0.0062 (6)0.0101 (6)
C4A0.0146 (7)0.0207 (7)0.0141 (6)0.0040 (5)0.0014 (5)0.0060 (6)
O4A0.0134 (5)0.0253 (6)0.0330 (6)0.0043 (4)0.0058 (4)0.0104 (5)
C5A0.0159 (7)0.0172 (6)0.0139 (6)0.0041 (5)0.0021 (5)0.0068 (5)
N5A0.0189 (6)0.0195 (6)0.0174 (6)0.0052 (5)0.0029 (5)0.0079 (5)
O5A0.0215 (6)0.0182 (5)0.0286 (6)0.0075 (4)0.0026 (4)0.0109 (5)
C6A0.0163 (7)0.0190 (7)0.0106 (6)0.0057 (5)0.0002 (5)0.0053 (5)
N6A0.0148 (6)0.0190 (6)0.0233 (6)0.0059 (5)0.0021 (5)0.0093 (5)
N1B0.0131 (6)0.0175 (6)0.0171 (6)0.0039 (4)0.0007 (4)0.0058 (5)
C2B0.0145 (7)0.0165 (6)0.0118 (6)0.0028 (5)0.0008 (5)0.0042 (5)
N2B0.0152 (6)0.0157 (6)0.0213 (6)0.0033 (4)0.0013 (5)0.0060 (5)
C21B0.0172 (7)0.0175 (7)0.0172 (6)0.0014 (5)0.0023 (5)0.0068 (6)
C22B0.0152 (7)0.0165 (6)0.0161 (6)0.0074 (5)0.0011 (5)0.0067 (5)
O21B0.0149 (5)0.0234 (5)0.0210 (5)0.0026 (4)0.0005 (4)0.0095 (4)
O22B0.0180 (6)0.0440 (7)0.0169 (5)0.0091 (5)0.0042 (4)0.0104 (5)
N3B0.0137 (6)0.0159 (6)0.0184 (6)0.0048 (4)0.0006 (5)0.0053 (5)
C3B0.0178 (7)0.0197 (7)0.0299 (8)0.0085 (6)0.0025 (6)0.0085 (6)
C4B0.0155 (7)0.0176 (7)0.0146 (6)0.0041 (5)0.0013 (5)0.0043 (5)
O4B0.0135 (5)0.0234 (5)0.0329 (6)0.0044 (4)0.0052 (4)0.0088 (5)
C5B0.0150 (7)0.0169 (6)0.0134 (6)0.0040 (5)0.0019 (5)0.0056 (5)
N5B0.0186 (6)0.0175 (6)0.0172 (6)0.0057 (5)0.0030 (5)0.0062 (5)
O5B0.0222 (6)0.0180 (5)0.0264 (5)0.0079 (4)0.0037 (4)0.0101 (4)
C6B0.0159 (7)0.0178 (6)0.0106 (6)0.0048 (5)0.0004 (5)0.0047 (5)
N6B0.0143 (6)0.0180 (6)0.0213 (6)0.0056 (5)0.0017 (5)0.0065 (5)
O10.0155 (5)0.0234 (5)0.0240 (5)0.0041 (4)0.0040 (4)0.0073 (5)
O20.0213 (6)0.0211 (5)0.0167 (5)0.0069 (4)0.0002 (4)0.0046 (4)
O30.0283 (7)0.0304 (6)0.0265 (6)0.0047 (5)0.0133 (5)0.0022 (5)
Geometric parameters (Å, º) top
Na1—O21A2.2731 (11)C6A—N6A1.3192 (18)
Na1—O5Ai2.3588 (11)N6A—H6A10.8800
Na1—O22.3657 (12)N6A—H6A20.8800
Na1—O12.4756 (12)N1B—C2B1.3305 (18)
Na1—O21Aii2.4918 (12)N1B—C6B1.3390 (18)
Na1—O32.8819 (15)C2B—N2B1.3316 (18)
Na1—Na1ii3.7020 (11)C2B—N3B1.3792 (18)
Na1—Na23.8838 (9)N2B—C21B1.4512 (18)
Na2—O32.3253 (13)N2B—H2B0.8800
Na2—O21Biii2.3591 (12)C21B—C22B1.5239 (19)
Na2—O21B2.3693 (11)C21B—H21C0.9900
Na2—O12.4040 (12)C21B—H21D0.9900
Na2—O5Biv2.4273 (12)C22B—O22B1.2462 (17)
Na2—Na2iii3.6914 (11)C22B—O21B1.2581 (17)
N1A—C2A1.3299 (18)C22B—Na2iii3.1296 (15)
N1A—C6A1.3413 (18)O21B—Na2iii2.3591 (11)
C2A—N2A1.3249 (18)N3B—C4B1.3984 (18)
C2A—N3A1.3825 (18)N3B—C3B1.4672 (18)
N2A—C21A1.4462 (18)C3B—H3B10.9800
N2A—H2A0.8800C3B—H3B20.9800
C21A—C22A1.5254 (19)C3B—H3B30.9800
C21A—H21A0.9900C4B—O4B1.2256 (18)
C21A—H21B0.9900C4B—C5B1.454 (2)
C22A—O21A1.2495 (17)C5B—N5B1.3330 (18)
C22A—O22A1.2524 (16)C5B—C6B1.4387 (19)
O21A—Na1ii2.4918 (12)N5B—O5B1.2832 (15)
N3A—C4A1.3946 (18)O5B—Na2i2.4273 (12)
N3A—C3A1.4688 (18)C6B—N6B1.3204 (18)
C3A—H3A10.9800N6B—H6B10.8800
C3A—H3A20.9800N6B—H6B20.8800
C3A—H3A30.9800O1—H110.958 (15)
C4A—O4A1.2272 (18)O1—H120.955 (12)
C4A—C5A1.4543 (19)O2—H210.961 (12)
C5A—N5A1.3311 (18)O2—H220.957 (6)
C5A—C6A1.4438 (19)O3—H310.960 (14)
N5A—O5A1.2817 (15)O3—H320.962 (16)
O5A—Na1iv2.3588 (11)
O21A—Na1—O5Ai131.98 (4)C6A—N6A—H6A1120.0
O21A—Na1—O2126.48 (4)C6A—N6A—H6A2120.0
O5Ai—Na1—O287.51 (4)H6A1—N6A—H6A2120.0
O21A—Na1—O1110.28 (4)C2B—N1B—C6B118.33 (12)
O5Ai—Na1—O1108.96 (4)N1B—C2B—N2B118.25 (13)
O2—Na1—O178.62 (4)N1B—C2B—N3B124.58 (12)
O21A—Na1—O21Aii78.14 (4)N2B—C2B—N3B117.16 (12)
O5Ai—Na1—O21Aii79.36 (4)C2B—N2B—C21B122.86 (12)
O2—Na1—O21Aii76.14 (4)C2B—N2B—H2B118.6
O1—Na1—O21Aii153.04 (4)C21B—N2B—H2B118.6
O21A—Na1—O392.13 (4)N2B—C21B—C22B114.43 (11)
O5Ai—Na1—O373.93 (4)N2B—C21B—H21C108.7
O2—Na1—O3138.44 (4)C22B—C21B—H21C108.7
O1—Na1—O373.15 (4)N2B—C21B—H21D108.7
O21Aii—Na1—O3133.29 (4)C22B—C21B—H21D108.7
O3—Na2—O21Biii122.66 (5)H21C—C21B—H21D107.6
O3—Na2—O21B119.87 (4)O22B—C22B—O21B125.19 (13)
O21Biii—Na2—O21B77.35 (4)O22B—C22B—C21B119.32 (12)
O3—Na2—O185.44 (5)O21B—C22B—C21B115.49 (12)
O21Biii—Na2—O1151.85 (5)O22B—C22B—Na2iii93.99 (9)
O21B—Na2—O190.38 (4)O21B—C22B—Na2iii42.44 (7)
O3—Na2—O5Biv116.79 (4)C21B—C22B—Na2iii135.42 (9)
O21Biii—Na2—O5Biv84.70 (4)C22B—O21B—Na2iii116.47 (9)
O21B—Na2—O5Biv121.43 (4)C22B—O21B—Na2129.49 (9)
O1—Na2—O5Biv80.27 (4)Na2iii—O21B—Na2102.65 (4)
C2A—N1A—C6A118.58 (12)C2B—N3B—C4B120.88 (12)
N2A—C2A—N1A118.46 (13)C2B—N3B—C3B120.83 (12)
N2A—C2A—N3A117.17 (12)C4B—N3B—C3B118.27 (12)
N1A—C2A—N3A124.36 (12)N3B—C3B—H3B1109.5
C2A—N2A—C21A122.94 (12)N3B—C3B—H3B2109.5
C2A—N2A—H2A118.5H3B1—C3B—H3B2109.5
C21A—N2A—H2A118.5N3B—C3B—H3B3109.5
N2A—C21A—C22A115.33 (11)H3B1—C3B—H3B3109.5
N2A—C21A—H21A108.4H3B2—C3B—H3B3109.5
C22A—C21A—H21A108.4O4B—C4B—N3B120.47 (13)
N2A—C21A—H21B108.4O4B—C4B—C5B124.38 (13)
C22A—C21A—H21B108.4N3B—C4B—C5B115.14 (12)
H21A—C21A—H21B107.5N5B—C5B—C6B127.06 (13)
O21A—C22A—O22A126.09 (13)N5B—C5B—C4B113.79 (13)
O21A—C22A—C21A114.96 (11)C6B—C5B—C4B119.14 (12)
O22A—C22A—C21A118.95 (12)O5B—N5B—C5B119.07 (12)
C22A—O21A—Na1135.07 (9)N5B—O5B—Na2i109.73 (8)
C22A—O21A—Na1ii123.05 (8)N6B—C6B—N1B118.10 (13)
Na1—O21A—Na1ii101.86 (4)N6B—C6B—C5B120.17 (12)
C2A—N3A—C4A121.00 (12)N1B—C6B—C5B121.73 (12)
C2A—N3A—C3A120.49 (12)C6B—N6B—H6B1120.0
C4A—N3A—C3A118.51 (12)C6B—N6B—H6B2120.0
N3A—C3A—H3A1109.5H6B1—N6B—H6B2120.0
N3A—C3A—H3A2109.5Na2—O1—Na1105.47 (4)
H3A1—C3A—H3A2109.5Na2—O1—H11114.7 (11)
N3A—C3A—H3A3109.5Na1—O1—H11106.9 (10)
H3A1—C3A—H3A3109.5Na2—O1—H1296.1 (11)
H3A2—C3A—H3A3109.5Na1—O1—H12125.7 (10)
O4A—C4A—N3A120.35 (13)H11—O1—H12108.0 (7)
O4A—C4A—C5A124.36 (13)Na1—O2—H2192.8 (10)
N3A—C4A—C5A115.29 (12)Na1—O2—H22110.4 (10)
N5A—C5A—C6A126.69 (13)H21—O2—H22107.5 (7)
N5A—C5A—C4A114.23 (13)Na2—O3—Na195.87 (4)
C6A—C5A—C4A119.05 (12)Na2—O3—H31123.9 (10)
O5A—N5A—C5A118.65 (12)Na1—O3—H3183.9 (12)
N5A—O5A—Na1iv118.26 (9)Na2—O3—H32124.6 (10)
N6A—C6A—N1A117.65 (13)Na1—O3—H32110.1 (13)
N6A—C6A—C5A120.91 (13)H31—O3—H32107.3 (7)
N1A—C6A—C5A121.41 (12)
C6A—N1A—C2A—N2A176.15 (12)O3—Na2—O21B—C22B20.38 (13)
C6A—N1A—C2A—N3A3.1 (2)O21Biii—Na2—O21B—C22B140.98 (13)
N1A—C2A—N2A—C21A3.7 (2)O1—Na2—O21B—C22B64.58 (12)
N3A—C2A—N2A—C21A177.01 (12)O5Biv—Na2—O21B—C22B143.39 (11)
C2A—N2A—C21A—C22A89.74 (16)C22Biii—Na2—O21B—C22B152.29 (10)
N2A—C21A—C22A—O21A171.76 (12)Na2iii—Na2—O21B—C22B140.98 (13)
N2A—C21A—C22A—O22A8.90 (18)Na1—Na2—O21B—C22B29.97 (12)
O22A—C22A—O21A—Na1162.20 (11)O3—Na2—O21B—Na2iii120.60 (6)
C21A—C22A—O21A—Na118.52 (19)O21Biii—Na2—O21B—Na2iii0.00 (4)
O22A—C22A—O21A—Na1ii19.5 (2)O1—Na2—O21B—Na2iii154.44 (5)
C21A—C22A—O21A—Na1ii159.79 (9)O5Biv—Na2—O21B—Na2iii75.63 (5)
O5Ai—Na1—O21A—C22A117.74 (13)C22Biii—Na2—O21B—Na2iii11.31 (4)
O2—Na1—O21A—C22A115.92 (13)Na1—Na2—O21B—Na2iii170.95 (4)
O1—Na1—O21A—C22A25.25 (14)N1B—C2B—N3B—C4B4.1 (2)
O21Aii—Na1—O21A—C22A178.55 (15)N2B—C2B—N3B—C4B176.91 (12)
O3—Na1—O21A—C22A47.56 (13)N1B—C2B—N3B—C3B174.44 (13)
Na1ii—Na1—O21A—C22A178.55 (15)N2B—C2B—N3B—C3B4.58 (19)
Na2—Na1—O21A—C22A12.82 (14)C2B—N3B—C4B—O4B179.18 (12)
O5Ai—Na1—O21A—Na1ii63.71 (7)C3B—N3B—C4B—O4B2.3 (2)
O2—Na1—O21A—Na1ii62.63 (6)C2B—N3B—C4B—C5B0.50 (19)
O1—Na1—O21A—Na1ii153.30 (5)C3B—N3B—C4B—C5B178.04 (12)
O21Aii—Na1—O21A—Na1ii0.00 (3)O4B—C4B—C5B—N5B1.7 (2)
O3—Na1—O21A—Na1ii133.89 (4)N3B—C4B—C5B—N5B177.92 (11)
Na2—Na1—O21A—Na1ii168.63 (3)O4B—C4B—C5B—C6B177.27 (13)
N2A—C2A—N3A—C4A174.77 (12)N3B—C4B—C5B—C6B3.06 (19)
N1A—C2A—N3A—C4A4.5 (2)C6B—C5B—N5B—O5B1.1 (2)
N2A—C2A—N3A—C3A5.84 (19)C4B—C5B—N5B—O5B180.00 (11)
N1A—C2A—N3A—C3A174.93 (13)C5B—N5B—O5B—Na2i174.01 (10)
C2A—N3A—C4A—O4A179.86 (12)C2B—N1B—C6B—N6B179.55 (12)
C3A—N3A—C4A—O4A0.7 (2)C2B—N1B—C6B—C5B0.4 (2)
C2A—N3A—C4A—C5A0.55 (19)N5B—C5B—C6B—N6B2.6 (2)
C3A—N3A—C4A—C5A178.86 (12)C4B—C5B—C6B—N6B176.25 (12)
O4A—C4A—C5A—N5A6.3 (2)N5B—C5B—C6B—N1B177.46 (13)
N3A—C4A—C5A—N5A174.11 (11)C4B—C5B—C6B—N1B3.7 (2)
O4A—C4A—C5A—C6A175.40 (13)O3—Na2—O1—Na12.11 (4)
N3A—C4A—C5A—C6A4.17 (19)O21Biii—Na2—O1—Na1179.01 (7)
C6A—C5A—N5A—O5A3.1 (2)O21B—Na2—O1—Na1117.83 (4)
C4A—C5A—N5A—O5A178.80 (11)O5Biv—Na2—O1—Na1120.30 (4)
C5A—N5A—O5A—Na1iv171.62 (9)C22Biii—Na2—O1—Na1143.05 (6)
C2A—N1A—C6A—N6A179.71 (12)Na2iii—Na2—O1—Na1136.91 (4)
C2A—N1A—C6A—C5A2.1 (2)O21A—Na1—O1—Na287.73 (5)
N5A—C5A—C6A—N6A5.8 (2)O5Ai—Na1—O1—Na264.04 (5)
C4A—C5A—C6A—N6A176.12 (12)O2—Na1—O1—Na2147.37 (5)
N5A—C5A—C6A—N1A172.33 (13)O21Aii—Na1—O1—Na2168.21 (7)
C4A—C5A—C6A—N1A5.7 (2)O3—Na1—O1—Na21.77 (4)
C6B—N1B—C2B—N2B177.41 (12)Na1ii—Na1—O1—Na2118.26 (6)
C6B—N1B—C2B—N3B3.6 (2)O21Biii—Na2—O3—Na1179.98 (4)
N1B—C2B—N2B—C21B0.1 (2)O21B—Na2—O3—Na186.06 (5)
N3B—C2B—N2B—C21B179.15 (12)O1—Na2—O3—Na11.75 (4)
C2B—N2B—C21B—C22B101.62 (15)O5Biv—Na2—O3—Na178.44 (5)
N2B—C21B—C22B—O22B13.31 (18)C22Biii—Na2—O3—Na1154.99 (4)
N2B—C21B—C22B—O21B166.48 (11)Na2iii—Na2—O3—Na1131.98 (5)
N2B—C21B—C22B—Na2iii146.45 (10)O21A—Na1—O3—Na2112.33 (4)
O22B—C22B—O21B—Na2iii49.83 (17)O5Ai—Na1—O3—Na2114.37 (5)
C21B—C22B—O21B—Na2iii130.40 (10)O2—Na1—O3—Na247.51 (8)
O22B—C22B—O21B—Na2173.51 (10)O1—Na1—O3—Na21.77 (4)
C21B—C22B—O21B—Na26.27 (17)O21Aii—Na1—O3—Na2172.01 (4)
Na2iii—C22B—O21B—Na2136.66 (14)Na1ii—Na1—O3—Na2145.19 (4)
Symmetry codes: (i) x1, y1, 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···AD—HH···AD···AD—H···A
N2A—H2A···O2v0.882.052.810 (2)144
N2B—H2B···O21Bvi0.882.433.187 (2)144
N6A—H6A1···O4Avii0.882.133.002 (2)169
N6A—H62A···O5A0.881.992.628 (2)128
N6B—H6B1···O4Bv0.882.092.953 (2)165
N6B—H6B2···O5B0.881.982.628 (2)129
O1—H11···O22Bvi0.96 (2)1.77 (2)2.711 (2)166 (1)
O1—H12···N5Biv0.96 (1)1.89 (1)2.738 (2)146 (1)
O2—H21···O22Aii0.96 (1)1.76 (1)2.691 (2)161 (1)
O2—H22···O22Bvi0.96 (1)1.83 (1)2.751 (2)161 (1)
O3—H31···N5Ai0.96 (1)1.87 (1)2.771 (2)156 (1)
O3—H32···O22Aviii0.96 (2)1.75 (2)2.708 (2)175 (1)
Symmetry codes: (i) x1, y1, z; (ii) x, y, z+1; (iv) x+1, y+1, z; (v) x+1, y, z; (vi) x, y, z+2; (vii) x1, 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
C7H10KN5O5F(000) = 584
Mr = 283.30Dx = 1.737 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 7.8114 (2) ÅCell parameters from 2814 reflections
b = 16.4811 (5) Åθ = 2.9–29.0°
c = 8.5560 (2) ŵ = 0.52 mm1
β = 100.408 (2)°T = 150 K
V = 1083.38 (5) Å3Block, red
Z = 40.10 × 0.10 × 0.05 mm
Data collection top
Kappa-CCD
diffractometer
2814 independent reflections
Radiation source: fine-focus sealed X-ray tube2226 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
ϕ scans and ω scans with κ offsetsθmax = 29.0°, θmin = 2.9°
Absorption correction: multi-scan
SORTAV (Blessing, 1995 & 1997)
h = 1010
Tmin = 0.950, Tmax = 0.975k = 1923
8482 measured reflectionsl = 1111
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-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 parametersΔρmax = 0.34 e Å3
3 restraintsΔρmin = 0.50 e Å3
Crystal data top
C7H10KN5O5V = 1083.38 (5) Å3
Mr = 283.30Z = 4
Monoclinic, P21/cMo Kα radiation
a = 7.8114 (2) ŵ = 0.52 mm1
b = 16.4811 (5) ÅT = 150 K
c = 8.5560 (2) Å0.10 × 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 = 0.975Rint = 0.046
8482 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0423 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.07Δρmax = 0.34 e Å3
2814 reflectionsΔρmin = 0.50 e Å3
170 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.46135 (5)0.25777 (2)0.69176 (4)0.01931 (14)
N10.17520 (19)0.40422 (9)0.56971 (16)0.0171 (3)
C20.1470 (2)0.42211 (10)0.41549 (19)0.0143 (3)
N20.05109 (18)0.37122 (9)0.31546 (16)0.0164 (3)
C210.0327 (2)0.30124 (10)0.3721 (2)0.0169 (4)
C220.0856 (2)0.22960 (10)0.42938 (19)0.0151 (3)
O210.23875 (16)0.22893 (8)0.40508 (14)0.0194 (3)
O220.01458 (16)0.17404 (7)0.49617 (14)0.0206 (3)
C30.1604 (3)0.50720 (11)0.1815 (2)0.0220 (4)
N30.20734 (18)0.49089 (8)0.35225 (15)0.0152 (3)
C40.3059 (2)0.54870 (10)0.4488 (2)0.0172 (4)
O40.35827 (17)0.60912 (7)0.38895 (15)0.0247 (3)
C50.3391 (2)0.53054 (10)0.6177 (2)0.0165 (4)
N50.4309 (2)0.58701 (9)0.70871 (17)0.0212 (3)
O50.47143 (17)0.57318 (8)0.85983 (14)0.0254 (3)
C60.2719 (2)0.45560 (10)0.67092 (19)0.0155 (3)
N60.3054 (2)0.43546 (9)0.82198 (17)0.0203 (3)
O10.66183 (17)0.30429 (8)0.97742 (14)0.0223 (3)
H20.03800.38010.21260.020*
H21A0.12520.28220.28520.020*
H21B0.08980.31900.46060.020*
H3A0.19980.46220.12200.033*
H3B0.21620.55760.15630.033*
H3C0.03380.51270.15190.033*
H6A0.26470.38970.85360.024*
H6B0.36840.46780.89150.024*
H110.7840 (8)0.3119 (10)0.980 (2)0.027*
H120.6177 (19)0.3529 (7)1.017 (2)0.027*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0193 (2)0.0210 (2)0.0180 (2)0.00012 (14)0.00447 (16)0.00195 (14)
N10.0203 (8)0.0161 (7)0.0149 (7)0.0019 (6)0.0033 (6)0.0007 (6)
C20.0156 (9)0.0111 (8)0.0171 (8)0.0025 (6)0.0052 (7)0.0008 (6)
N20.0191 (8)0.0154 (7)0.0140 (7)0.0023 (6)0.0010 (6)0.0016 (5)
C210.0144 (8)0.0146 (8)0.0210 (8)0.0021 (6)0.0013 (7)0.0012 (7)
C220.0169 (9)0.0150 (8)0.0121 (7)0.0019 (7)0.0008 (6)0.0035 (6)
O210.0167 (6)0.0213 (7)0.0208 (6)0.0005 (5)0.0045 (5)0.0029 (5)
O220.0214 (7)0.0186 (7)0.0219 (6)0.0010 (5)0.0038 (5)0.0055 (5)
C30.0297 (11)0.0193 (9)0.0169 (8)0.0024 (8)0.0037 (7)0.0026 (7)
N30.0186 (8)0.0122 (7)0.0152 (7)0.0007 (6)0.0041 (6)0.0004 (5)
C40.0166 (9)0.0134 (8)0.0225 (9)0.0008 (7)0.0064 (7)0.0013 (7)
O40.0312 (8)0.0164 (7)0.0273 (7)0.0072 (5)0.0078 (6)0.0017 (5)
C50.0162 (9)0.0127 (8)0.0210 (8)0.0013 (6)0.0043 (7)0.0015 (7)
N50.0207 (8)0.0181 (8)0.0239 (8)0.0022 (6)0.0009 (6)0.0030 (6)
O50.0280 (8)0.0223 (7)0.0228 (7)0.0019 (6)0.0034 (6)0.0055 (5)
C60.0141 (8)0.0151 (8)0.0179 (8)0.0022 (6)0.0049 (6)0.0014 (7)
N60.0249 (8)0.0190 (8)0.0164 (7)0.0036 (6)0.0021 (6)0.0006 (6)
O10.0215 (7)0.0217 (7)0.0247 (7)0.0001 (5)0.0066 (5)0.0016 (5)
Geometric parameters (Å, º) top
K1—O21i2.7476 (12)C3—N31.466 (2)
K1—O4ii2.7616 (13)C3—H3A0.9800
K1—O12.7624 (13)C3—H3B0.9800
K1—O212.7794 (12)C3—H3C0.9800
K1—O1iii2.8106 (13)N3—C41.398 (2)
K1—N5iv3.0157 (15)C4—O41.223 (2)
K1—O5iv3.1320 (13)C4—C51.453 (2)
N1—C21.331 (2)O4—K1ii2.7616 (13)
N1—C61.342 (2)C5—N51.336 (2)
C2—N21.329 (2)C5—C61.447 (2)
C2—N31.375 (2)N5—O51.2946 (19)
N2—C211.452 (2)N5—K1v3.0157 (15)
N2—H20.8800O5—K1v3.1320 (13)
C21—C221.524 (2)C6—N61.314 (2)
C21—H21A0.9900N6—H6A0.8800
C21—H21B0.9900N6—H6B0.8800
C22—O211.251 (2)O1—K1i2.8106 (13)
C22—O221.260 (2)O1—H110.959 (7)
O21—K1iii2.7476 (12)O1—H120.958 (13)
O21i—K1—O4ii121.03 (4)C22—K1—K1iii59.13 (3)
O21i—K1—O173.49 (4)N6—K1—K1iii116.03 (3)
O4ii—K1—O176.55 (4)K1i—K1—K1iii173.15 (2)
O21i—K1—O21103.28 (4)C2—N1—C6118.23 (14)
O4ii—K1—O21100.44 (4)C2—N1—K1116.96 (10)
O1—K1—O21173.01 (4)C6—N1—K189.27 (10)
O21i—K1—O1iii163.04 (4)N2—C2—N1118.15 (15)
O4ii—K1—O1iii75.90 (4)N2—C2—N3117.40 (14)
O1—K1—O1iii112.63 (5)N1—C2—N3124.44 (15)
O21—K1—O1iii72.27 (4)C2—N2—C21121.47 (13)
O21i—K1—N5iv93.71 (4)C2—N2—H2119.3
O4ii—K1—N5iv133.08 (4)C21—N2—H2119.3
O1—K1—N5iv85.67 (4)N2—C21—C22116.06 (14)
O21—K1—N5iv100.82 (4)N2—C21—H21A108.3
O1iii—K1—N5iv71.62 (4)C22—C21—H21A108.3
O21i—K1—O5iv108.26 (4)N2—C21—H21B108.3
O4ii—K1—O5iv129.07 (4)C22—C21—H21B108.3
O1—K1—O5iv108.16 (4)H21A—C21—H21B107.4
O21—K1—O5iv78.67 (4)O21—C22—O22125.57 (16)
O1iii—K1—O5iv55.05 (4)O21—C22—C21119.71 (15)
N5iv—K1—O5iv24.22 (4)O22—C22—C21114.70 (15)
O21i—K1—N171.38 (4)O21—C22—K151.06 (8)
O4ii—K1—N171.90 (4)O22—C22—K1101.46 (10)
O1—K1—N1108.52 (4)C21—C22—K1120.58 (10)
O21—K1—N164.49 (4)C22—O21—K1iii148.09 (11)
O1iii—K1—N1118.76 (4)C22—O21—K1108.45 (10)
N5iv—K1—N1154.56 (4)K1iii—O21—K1101.68 (4)
O5iv—K1—N1141.32 (4)N3—C3—H3A109.5
O21i—K1—C2282.80 (4)N3—C3—H3B109.5
O4ii—K1—C22111.29 (4)H3A—C3—H3B109.5
O1—K1—C22155.32 (4)N3—C3—H3C109.5
O21—K1—C2220.49 (4)H3A—C3—H3C109.5
O1iii—K1—C2292.06 (4)H3B—C3—H3C109.5
N5iv—K1—C22102.90 (4)C2—N3—C4121.38 (13)
O5iv—K1—C2285.46 (4)C2—N3—C3120.11 (14)
N1—K1—C2255.89 (4)C4—N3—C3118.42 (14)
O21i—K1—N654.00 (4)O4—C4—N3119.85 (15)
O4ii—K1—N668.32 (4)O4—C4—C5124.83 (16)
O1—K1—N669.75 (4)N3—C4—C5115.32 (14)
O21—K1—N6103.30 (4)C4—O4—K1ii167.28 (12)
O1iii—K1—N6142.58 (4)N5—C5—C6126.76 (15)
N5iv—K1—N6143.27 (4)N5—C5—C4114.61 (15)
O5iv—K1—N6162.25 (4)C6—C5—C4118.63 (15)
N1—K1—N639.24 (3)O5—N5—C5117.89 (15)
C22—K1—N690.92 (4)O5—N5—K1v82.93 (9)
O21i—K1—K1i39.43 (3)C5—N5—K1v155.18 (12)
O4ii—K1—K1i112.90 (3)N5—O5—K1v72.85 (9)
O1—K1—K1i40.15 (3)N6—C6—N1117.65 (16)
O21—K1—K1i139.28 (3)N6—C6—C5120.39 (15)
O1iii—K1—K1i136.89 (3)N1—C6—C5121.96 (15)
N5iv—K1—K1i73.30 (3)C6—N6—K185.15 (10)
O5iv—K1—K1i96.48 (3)C6—N6—H6A120.0
N1—K1—K1i103.62 (3)K1—N6—H6A62.4
C22—K1—K1i119.79 (3)C6—N6—H6B120.0
N6—K1—K1i70.31 (3)K1—N6—H6B123.2
O21i—K1—K1iii141.44 (3)H6A—N6—H6B120.0
O4ii—K1—K1iii72.89 (3)K1—O1—K1i100.53 (4)
O1—K1—K1iii142.90 (3)K1—O1—H11117.5 (11)
O21—K1—K1iii38.89 (3)K1i—O1—H11134.4 (12)
O1iii—K1—K1iii39.33 (3)K1—O1—H12111.2 (11)
N5iv—K1—K1iii100.12 (3)K1i—O1—H1278.2 (11)
O5iv—K1—K1iii76.76 (2)H11—O1—H12107.5 (7)
N1—K1—K1iii81.44 (2)
O21i—K1—N1—C2156.46 (12)C21—C22—O21—K1106.98 (14)
O4ii—K1—N1—C270.52 (12)O21i—K1—O21—C221.44 (10)
O1—K1—N1—C2138.96 (11)O4ii—K1—O21—C22124.15 (11)
O21—K1—N1—C241.03 (11)O1iii—K1—O21—C22164.45 (12)
O1iii—K1—N1—C28.66 (13)N5iv—K1—O21—C2297.91 (11)
N5iv—K1—N1—C299.78 (14)O5iv—K1—O21—C22107.77 (11)
O5iv—K1—N1—C260.24 (13)N1—K1—O21—C2260.13 (11)
C22—K1—N1—C262.53 (11)N6—K1—O21—C2254.17 (11)
N6—K1—N1—C2148.15 (14)K1i—K1—O21—C2220.99 (13)
K1i—K1—N1—C2179.48 (11)K1iii—K1—O21—C22169.33 (13)
K1iii—K1—N1—C24.19 (11)O21i—K1—O21—K1iii170.77 (5)
O21i—K1—N1—C681.93 (10)O4ii—K1—O21—K1iii45.18 (5)
O4ii—K1—N1—C651.09 (9)O1iii—K1—O21—K1iii26.22 (4)
O1—K1—N1—C617.35 (10)N5iv—K1—O21—K1iii92.75 (4)
O21—K1—N1—C6162.64 (10)O5iv—K1—O21—K1iii82.90 (4)
O1iii—K1—N1—C6112.95 (10)N1—K1—O21—K1iii109.21 (5)
N5iv—K1—N1—C6138.61 (11)C22—K1—O21—K1iii169.33 (13)
O5iv—K1—N1—C6178.15 (9)N6—K1—O21—K1iii115.16 (4)
C22—K1—N1—C6175.85 (11)K1i—K1—O21—K1iii169.67 (3)
N6—K1—N1—C626.54 (9)N2—C2—N3—C4178.58 (15)
K1i—K1—N1—C658.90 (9)N1—C2—N3—C40.1 (2)
K1iii—K1—N1—C6125.80 (9)N2—C2—N3—C32.1 (2)
C6—N1—C2—N2179.94 (15)N1—C2—N3—C3176.42 (16)
K1—N1—C2—N275.19 (17)C2—N3—C4—O4179.74 (15)
C6—N1—C2—N31.4 (2)C3—N3—C4—O43.7 (2)
K1—N1—C2—N3106.31 (15)C2—N3—C4—C50.1 (2)
N1—C2—N2—C214.8 (2)C3—N3—C4—C5176.64 (14)
N3—C2—N2—C21173.85 (14)N3—C4—O4—K1ii146.9 (4)
C2—N2—C21—C2276.0 (2)C5—C4—O4—K1ii32.8 (6)
N2—C21—C22—O2110.0 (2)O4—C4—C5—N51.4 (3)
N2—C21—C22—O22171.48 (14)N3—C4—C5—N5178.92 (15)
N2—C21—C22—K149.76 (18)O4—C4—C5—C6178.60 (16)
O21i—K1—C22—O21178.59 (10)N3—C4—C5—C61.0 (2)
O4ii—K1—C22—O2160.86 (12)C6—C5—N5—O52.9 (3)
O1—K1—C22—O21165.35 (11)C4—C5—N5—O5177.18 (14)
O1iii—K1—C22—O2114.80 (11)C6—C5—N5—K1v141.5 (2)
N5iv—K1—C22—O2186.42 (11)C4—C5—N5—K1v38.5 (3)
O5iv—K1—C22—O2169.50 (11)C5—N5—O5—K1v165.73 (15)
N1—K1—C22—O21109.06 (12)C2—N1—C6—N6177.01 (15)
N6—K1—C22—O21127.89 (11)K1—N1—C6—N656.49 (14)
K1i—K1—C22—O21164.38 (10)C2—N1—C6—C52.6 (2)
K1iii—K1—C22—O217.78 (10)K1—N1—C6—C5123.12 (15)
O21i—K1—C22—O2251.77 (10)N5—C5—C6—N62.9 (3)
O4ii—K1—C22—O22172.32 (10)C4—C5—C6—N6177.14 (15)
O1—K1—C22—O2267.83 (15)N5—C5—C6—N1177.47 (16)
O21—K1—C22—O22126.82 (17)C4—C5—C6—N12.5 (2)
O1iii—K1—C22—O22112.02 (10)N1—C6—N6—K154.16 (14)
N5iv—K1—C22—O2240.41 (11)C5—C6—N6—K1125.46 (14)
O5iv—K1—C22—O2257.32 (10)O21i—K1—N6—C6132.66 (11)
N1—K1—C22—O22124.12 (12)O4ii—K1—N6—C660.35 (10)
N6—K1—C22—O22105.29 (10)O1—K1—N6—C6143.45 (11)
K1i—K1—C22—O2237.56 (11)O21—K1—N6—C635.76 (10)
K1iii—K1—C22—O22134.60 (11)O1iii—K1—N6—C642.35 (13)
O21i—K1—C22—C2176.19 (12)N5iv—K1—N6—C6165.51 (9)
O4ii—K1—C22—C2144.36 (13)O5iv—K1—N6—C6130.15 (13)
O1—K1—C22—C2160.13 (17)N1—K1—N6—C627.25 (9)
O21—K1—C22—C21105.22 (17)C22—K1—N6—C652.25 (10)
O1iii—K1—C22—C21120.02 (12)K1i—K1—N6—C6173.71 (10)
N5iv—K1—C22—C21168.36 (12)K1iii—K1—N6—C63.47 (11)
O5iv—K1—C22—C21174.73 (12)O21i—K1—O1—K1i26.09 (4)
N1—K1—C22—C213.84 (11)O4ii—K1—O1—K1i154.68 (5)
N6—K1—C22—C2122.67 (12)O1iii—K1—O1—K1i137.10 (5)
K1i—K1—C22—C2190.40 (12)N5iv—K1—O1—K1i69.07 (4)
K1iii—K1—C22—C2197.44 (12)O5iv—K1—O1—K1i78.20 (5)
O22—C22—O21—K1iii125.35 (19)N1—K1—O1—K1i89.32 (4)
C21—C22—O21—K1iii53.0 (3)C22—K1—O1—K1i42.73 (11)
K1—C22—O21—K1iii159.9 (2)N6—K1—O1—K1i83.13 (4)
O22—C22—O21—K174.70 (18)K1iii—K1—O1—K1i170.15 (3)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1, y+1, z+1; (iii) x, y+1/2, z1/2; (iv) x+1, y1/2, z+3/2; (v) x+1, y+1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O22iii0.882.032.796 (2)144
N6—H6A···O21i0.882.022.872 (2)162
N6—H6B···O50.881.952.605 (2)130
O1—H11···O22vi0.96 (1)1.80 (1)2.754 (2)177 (2)
O1—H12···O5vii0.96 (1)1.83 (1)2.761 (2)164 (1)
Symmetry codes: (i) x, y+1/2, z+1/2; (iii) x, y+1/2, z1/2; (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 = 687.46F(000) = 359
Triclinic, P1Dx = 1.629 Mg m3
a = 7.4476 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.2351 (4) ÅCell parameters from 3131 reflections
c = 12.6372 (5) Åθ = 1.7–27.5°
α = 105.258 (2)°µ = 0.57 mm1
β = 92.153 (3)°T = 150 K
γ = 108.94 (2)°Plate, red
V = 700.81 (5) Å30.45 × 0.35 × 0.08 mm
Data collection top
Kappa-CCD
diffractometer
3131 independent reflections
Radiation source: fine-focus sealed X-ray tube2814 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.068
ϕ scans and ω scans with κ offsetsθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan
SORTAV (Blessing, 1995 & 1997)
h = 99
Tmin = 0.784, Tmax = 0.959k = 1010
7489 measured reflectionsl = 1516
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-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 parametersΔρmax = 0.50 e Å3
15 restraintsΔρmin = 0.57 e Å3
Crystal data top
C14H24MnN10O12·6(H2O)γ = 108.94 (2)°
Mr = 687.46V = 700.81 (5) Å3
Triclinic, P1Z = 1
a = 7.4476 (3) ÅMo Kα radiation
b = 8.2351 (4) ŵ = 0.57 mm1
c = 12.6372 (5) ÅT = 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 = 0.959Rint = 0.068
7489 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04015 restraints
wR(F2) = 0.107H-atom parameters constrained
S = 1.10Δρmax = 0.50 e Å3
3131 reflectionsΔρmin = 0.57 e Å3
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
xyzUiso*/Ueq
Mn10.50000.00000.50000.01698 (13)
N10.1453 (2)0.1486 (2)0.91956 (13)0.0187 (3)
C20.0347 (3)0.0625 (2)0.87141 (15)0.0173 (4)
N20.0704 (2)0.0790 (2)0.78329 (13)0.0197 (3)
C210.0819 (3)0.1344 (3)0.73489 (16)0.0206 (4)
C220.1847 (2)0.0280 (2)0.65941 (14)0.0171 (4)
O210.32251 (18)0.07366 (18)0.62267 (11)0.0211 (3)
O220.13010 (19)0.08985 (18)0.63825 (11)0.0219 (3)
C30.3836 (3)0.0089 (3)0.84736 (17)0.0247 (4)
N30.1892 (2)0.1080 (2)0.90783 (13)0.0184 (3)
C40.1650 (3)0.2478 (3)1.00356 (15)0.0187 (4)
O40.3040 (2)0.2836 (2)1.03735 (12)0.0269 (3)
C50.0298 (3)0.3443 (3)1.05824 (15)0.0179 (4)
N50.0466 (2)0.4789 (2)1.14923 (13)0.0217 (3)
O50.2152 (2)0.5711 (2)1.20237 (12)0.0270 (3)
C60.1810 (3)0.2877 (3)1.01120 (15)0.0178 (4)
N60.3591 (2)0.3701 (2)1.05951 (14)0.0226 (3)
O1W0.4172 (2)0.23277 (18)0.52434 (12)0.0241 (3)
O2W0.2367 (2)0.1481 (2)0.37756 (12)0.0276 (3)
O3W0.3797 (2)0.36643 (19)0.35193 (13)0.0294 (3)
O4W0.1927 (3)0.5302 (3)0.5202 (2)0.0554 (6)
O5W0.6924 (3)0.5341 (2)0.25271 (16)0.0458 (5)
H20.18990.14110.75330.024*
H21A0.02710.26270.69190.025*
H21B0.17740.12320.79550.025*
H3A0.38150.00220.76890.037*
H3B0.47040.07120.87790.037*
H3C0.42820.11270.85510.037*
H6A0.45080.33381.03170.027*
H6B0.38670.46171.11970.027*
H1W10.2982 (17)0.206 (3)0.5541 (16)0.029*
H2W10.402 (3)0.275 (3)0.4621 (13)0.029*
H1W20.121 (2)0.121 (3)0.377 (2)0.043 (7)*
H2W20.210 (4)0.266 (2)0.328 (2)0.084 (12)*
H1W30.494 (3)0.434 (3)0.329 (3)0.087 (12)*
H2W30.323 (4)0.449 (3)0.392 (3)0.077 (11)*
H1W40.067 (3)0.511 (5)0.488 (4)0.135 (19)*
H2W40.258 (5)0.6570 (12)0.550 (3)0.104 (15)*
H1W50.762 (3)0.480 (3)0.2016 (19)0.055*
H2W50.769 (3)0.6574 (13)0.286 (2)0.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0180 (2)0.0183 (2)0.0164 (2)0.00734 (15)0.00728 (14)0.00576 (15)
N10.0156 (7)0.0238 (8)0.0203 (8)0.0099 (6)0.0075 (6)0.0079 (6)
C20.0173 (8)0.0234 (9)0.0178 (8)0.0099 (7)0.0087 (7)0.0122 (7)
N20.0163 (7)0.0247 (8)0.0194 (8)0.0074 (6)0.0081 (6)0.0077 (7)
C210.0210 (9)0.0234 (9)0.0212 (9)0.0104 (7)0.0105 (7)0.0083 (7)
C220.0151 (8)0.0195 (9)0.0137 (8)0.0038 (7)0.0028 (6)0.0026 (7)
O210.0198 (6)0.0285 (7)0.0204 (7)0.0115 (5)0.0098 (5)0.0108 (6)
O220.0223 (7)0.0236 (7)0.0244 (7)0.0103 (5)0.0090 (5)0.0106 (6)
C30.0155 (9)0.0340 (11)0.0248 (10)0.0097 (8)0.0044 (7)0.0075 (8)
N30.0145 (7)0.0254 (8)0.0189 (8)0.0091 (6)0.0067 (6)0.0088 (6)
C40.0197 (9)0.0265 (9)0.0179 (9)0.0137 (7)0.0084 (7)0.0117 (8)
O40.0200 (7)0.0376 (8)0.0275 (7)0.0169 (6)0.0095 (6)0.0069 (6)
C50.0189 (9)0.0240 (9)0.0174 (8)0.0118 (7)0.0073 (7)0.0106 (7)
N50.0236 (8)0.0266 (8)0.0199 (8)0.0130 (7)0.0055 (6)0.0092 (7)
O50.0240 (7)0.0308 (8)0.0236 (7)0.0108 (6)0.0021 (6)0.0019 (6)
C60.0175 (8)0.0242 (9)0.0180 (8)0.0103 (7)0.0071 (7)0.0119 (7)
N60.0159 (7)0.0290 (9)0.0237 (8)0.0111 (6)0.0047 (6)0.0047 (7)
O1W0.0269 (7)0.0226 (7)0.0280 (7)0.0124 (6)0.0112 (6)0.0100 (6)
O2W0.0214 (7)0.0315 (8)0.0244 (7)0.0103 (6)0.0007 (6)0.0020 (6)
O3W0.0343 (8)0.0224 (7)0.0306 (8)0.0082 (6)0.0051 (6)0.0079 (6)
O4W0.0279 (9)0.0410 (11)0.1016 (18)0.0133 (8)0.0171 (10)0.0247 (11)
O5W0.0495 (10)0.0259 (8)0.0551 (11)0.0082 (7)0.0353 (9)0.0028 (8)
Geometric parameters (Å, º) top
Mn1—O1W2.1498 (13)C3—H3C0.9800
Mn1—O1Wi2.1498 (13)N3—C41.392 (2)
Mn1—O21i2.1555 (12)C4—O41.227 (2)
Mn1—O212.1556 (12)C4—C51.449 (3)
Mn1—O2W2.2254 (14)C5—N51.340 (3)
Mn1—O2Wi2.2254 (15)C5—C61.444 (2)
N1—C21.328 (2)N5—O51.286 (2)
N1—C61.344 (2)C6—N61.315 (2)
C2—N21.327 (3)N6—H6A0.8800
C2—N31.381 (2)N6—H6B0.8800
N2—C211.452 (2)O1W—H1W10.96 (2)
N2—H20.8800O1W—H2W10.96 (2)
C21—C221.524 (2)O2W—H1W20.96 (2)
C21—H21A0.9900O2W—H2W20.96 (2)
C21—H21B0.9900O3W—H1W30.96 (3)
C22—O221.250 (2)O3W—H2W30.96 (3)
C22—O211.267 (2)O4W—H1W40.95 (3)
C3—N31.472 (2)O4W—H2W40.96 (2)
C3—H3A0.9800O5W—H1W50.95 (2)
C3—H3B0.9800O5W—H2W50.96 (2)
O1W—Mn1—O1Wi180.0N3—C3—H3A109.5
O1W—Mn1—O21i91.84 (5)N3—C3—H3B109.5
O1Wi—Mn1—O21i88.16 (5)H3A—C3—H3B109.5
O1W—Mn1—O2188.16 (5)N3—C3—H3C109.5
O1Wi—Mn1—O2191.84 (5)H3A—C3—H3C109.5
O21i—Mn1—O21180.0H3B—C3—H3C109.5
O1W—Mn1—O2W87.15 (6)C2—N3—C4120.64 (16)
O1Wi—Mn1—O2W92.85 (6)C2—N3—C3120.96 (16)
O21i—Mn1—O2W93.72 (5)C4—N3—C3118.39 (15)
O21—Mn1—O2W86.28 (5)O4—C4—N3120.23 (17)
O1W—Mn1—O2Wi92.85 (6)O4—C4—C5123.57 (17)
O1Wi—Mn1—O2Wi87.15 (6)N3—C4—C5116.20 (15)
O21i—Mn1—O2Wi86.28 (5)N5—C5—C6127.45 (17)
O21—Mn1—O2Wi93.72 (5)N5—C5—C4114.18 (15)
O2W—Mn1—O2Wi180.0C6—C5—C4118.37 (16)
C2—N1—C6118.46 (15)O5—N5—C5117.91 (15)
N2—C2—N1118.28 (16)N6—C6—N1118.07 (16)
N2—C2—N3117.25 (16)N6—C6—C5120.10 (17)
N1—C2—N3124.45 (17)N1—C6—C5121.81 (17)
C2—N2—C21121.97 (16)C6—N6—H6A120.0
C2—N2—H2119.0C6—N6—H6B120.0
C21—N2—H2119.0H6A—N6—H6B120.0
N2—C21—C22114.76 (15)Mn1—O1W—H1W1106.8 (13)
N2—C21—H21A108.6Mn1—O1W—H2W1118.6 (14)
C22—C21—H21A108.6H1W1—O1W—H2W1108 (2)
N2—C21—H21B108.6Mn1—O2W—H1W2126.6 (14)
C22—C21—H21B108.6Mn1—O2W—H2W2124.1 (15)
H21A—C21—H21B107.6H1W2—O2W—H2W2108 (2)
O22—C22—O21126.21 (16)H1W3—O3W—H2W3108 (2)
O22—C22—C21120.52 (15)H1W4—O4W—H2W4108 (3)
O21—C22—C21113.27 (16)H1W5—O5W—H2W5109 (2)
C22—O21—Mn1131.54 (12)
C6—N1—C2—N2177.54 (16)C2—N3—C4—O4177.60 (16)
C6—N1—C2—N31.3 (3)C3—N3—C4—O41.7 (3)
N1—C2—N2—C213.8 (3)C2—N3—C4—C52.4 (2)
N3—C2—N2—C21177.24 (15)C3—N3—C4—C5178.33 (16)
C2—N2—C21—C2280.4 (2)O4—C4—C5—N50.7 (3)
N2—C21—C22—O223.8 (3)N3—C4—C5—N5179.25 (15)
N2—C21—C22—O21176.85 (15)O4—C4—C5—C6179.13 (17)
O22—C22—O21—Mn17.5 (3)N3—C4—C5—C60.9 (2)
C21—C22—O21—Mn1171.83 (12)C6—C5—N5—O50.2 (3)
O1W—Mn1—O21—C2220.30 (16)C4—C5—N5—O5179.93 (15)
O1Wi—Mn1—O21—C22159.70 (16)C2—N1—C6—N6178.78 (16)
O2W—Mn1—O21—C2266.96 (16)C2—N1—C6—C50.3 (3)
O2Wi—Mn1—O21—C22113.04 (16)N5—C5—C6—N60.9 (3)
N2—C2—N3—C4176.06 (15)C4—C5—C6—N6178.90 (16)
N1—C2—N3—C42.8 (3)N5—C5—C6—N1179.34 (17)
N2—C2—N3—C33.2 (2)C4—C5—C6—N10.5 (3)
N1—C2—N3—C3177.98 (17)
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3Wii0.882.022.804 (2)148
N6—H6A···O4iii0.882.002.828 (2)156
N6—H6B···O50.881.972.620 (2)130
O1W—H1W1···O220.96 (2)1.86 (2)2.742 (2)151 (2)
O1W—H2W1···O3W0.96 (2)1.77 (2)2.731 (2)177 (2)
O2W—H1W2···O22ii0.96 (2)1.98 (2)2.933 (2)174 (2)
O2W—H2W2···O5iv0.96 (2)1.80 (2)2.705 (2)156 (2)
O3W—H1W3···O5W0.96 (3)1.88 (3)2.817 (3)167 (3)
O3W—H2W3···O4W0.96 (3)2.00 (3)2.865 (3)150 (3)
O4W—H1W4···O4Wv0.95 (3)1.85 (3)2.754 (3)158 (4)
O4W—H2W4···O21vi0.96 (2)2.05 (2)2.981 (3)164 (3)
O5W—H1W5···O4vii0.95 (2)2.19 (2)2.958 (2)137 (2)
O5W—H1W5···N5vii0.95 (2)2.24 (2)3.100 (3)148 (2)
O5W—H2W5···O22viii0.96 (2)1.92 (2)2.864 (2)167 (2)
Symmetry codes: (ii) x, y, z+1; (iii) x+1, y, z; (iv) x, y1, z1; (v) x, y+1, z+1; (vi) x, y+1, z; (vii) x+1, y, z1; (viii) x+1, y+1, z+1.

Experimental details

(1)(190)(3)(MnL2)
Crystal data
Chemical formulaC7H14LiN5O7C14H22N10Na2O11C7H10KN5O5C14H24MnN10O12·6(H2O)
Mr287.17552.40283.30687.46
Crystal system, space groupMonoclinic, C2/cTriclinic, P1Monoclinic, P21/cTriclinic, P1
Temperature (K)150150150150
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), 90104.4350 (8), 97.8415 (8), 103.5004 (7)90, 100.408 (2), 90105.258 (2), 92.153 (3), 108.94 (2)
V3)2419.20 (14)1074.95 (3)1083.38 (5)700.81 (5)
Z8241
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.140.180.520.57
Crystal size (mm)0.20 × 0.10 × 0.100.45 × 0.25 × 0.050.10 × 0.10 × 0.050.45 × 0.35 × 0.08
Data collection
DiffractometerKappa-CCD
diffractometer
Kappa-CCD
diffractometer
Kappa-CCD
diffractometer
Kappa-CCD
diffractometer
Absorption correctionMulti-scan
SORTAV (Blessing, 1995 & 1997)
Multi-scan
SORTAV (Blessing, 1995 & 1997)
Multi-scan
SORTAV (Blessing, 1995 & 1997)
Multi-scan
SORTAV (Blessing, 1995 & 1997)
Tmin, Tmax0.973, 0.9860.924, 0.9910.950, 0.9750.784, 0.959
No. of measured, independent and
observed [I > 2σ(I)] reflections
7232, 2637, 2024 15704, 5449, 4455 8482, 2814, 2226 7489, 3131, 2814
Rint0.0270.0530.0460.068
(sin θ/λ)max1)0.6490.6820.6820.649
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 reflections2637544928143131
No. of parameters200354170233
No. of restraints99315
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.24, 0.300.35, 0.450.34, 0.500.50, 0.57

Computer programs: Kappa-CCD server software (Nonius, 1997), DENZO (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997b), ORTEP (Johnson, 1976), PLATON (Spek, 2000), SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).

Hydrogen-bond geometry (Å, º) for (MnL2) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3Wi0.882.022.804 (2)148
N6—H6A···O4ii0.882.002.828 (2)156
N6—H6B···O50.881.972.620 (2)130
O1W—H1W1···O220.96 (2)1.86 (2)2.742 (2)151 (2)
O1W—H2W1···O3W0.96 (2)1.77 (2)2.731 (2)177 (2)
O2W—H1W2···O22i0.96 (2)1.98 (2)2.933 (2)174 (2)
O2W—H2W2···O5iii0.96 (2)1.80 (2)2.705 (2)156 (2)
O3W—H1W3···O5W0.96 (3)1.88 (3)2.817 (3)167 (3)
O3W—H2W3···O4W0.96 (3)2.00 (3)2.865 (3)150 (3)
O4W—H1W4···O4Wiv0.95 (3)1.85 (3)2.754 (3)158 (4)
O4W—H2W4···O21v0.96 (2)2.05 (2)2.981 (3)164 (3)
O5W—H1W5···O4vi0.95 (2)2.19 (2)2.958 (2)137 (2)
O5W—H1W5···N5vi0.95 (2)2.24 (2)3.100 (3)148 (2)
O5W—H2W5···O22vii0.96 (2)1.92 (2)2.864 (2)167 (2)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z; (iii) x, y1, z1; (iv) x, y+1, z+1; (v) x, y+1, z; (vi) x+1, y, z1; (vii) x+1, y+1, z+1.
 

Subscribe to Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. B
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds