The title compound, 3K+·C2HN4O63-·2.5H2O, contains two diazeniumdiolate substituents which are nearly planar, with observed N-O and N-N double-bond distances in the range 1.276 (3)-1.309 (3) Å, revealing extensive double-bond delocalization over the four-atom groups. One water molecule lies on a twofold rotation axis.
Supporting information
CCDC reference: 271830
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.004 Å
- R factor = 0.037
- wR factor = 0.098
- Data-to-parameter ratio = 11.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............ 24.99 Deg.
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT213_ALERT_2_C Atom O3 has ADP max/min Ratio ............. 3.50 prolat
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.37 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3
PLAT731_ALERT_1_C Bond Calc 0.83(3), Rep 0.828(10) ...... 3.00 su-Rat
O1W -H1W 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.83(3), Rep 0.830(10) ...... 3.00 su-Rat
O2W -H2W 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.82(3), Rep 0.824(10) ...... 3.00 su-Rat
O2W -H3W 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.83(3), Rep 0.828(10) ...... 3.00 su-Rat
O1W -H1W 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.83(3), Rep 0.830(10) ...... 3.00 su-Rat
O2W -H2W 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.85(3), Rep 1.847(14) ...... 2.14 su-Rat
H2W -O3 1.555 5.656
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.97 Ratio
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 36.30 Deg.
O6 -C2 -K1 1.555 1.555 1.555
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
4 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Tripotassium ethanoate-2,2-diylbis(diazeniumdiolate) 2.5-hydrate
top
Crystal data top
3K+·C2HN4O63−·2.5H2O | F(000) = 1368 |
Mr = 339.41 | Dx = 1.978 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 27 reflections |
a = 28.831 (3) Å | θ = 5.0–12.5° |
b = 9.3063 (12) Å | µ = 1.24 mm−1 |
c = 8.6456 (12) Å | T = 173 K |
β = 100.642 (10)° | Rectangular prism, colorless |
V = 2279.8 (5) Å3 | 0.32 × 0.24 × 0.10 mm |
Z = 8 | |
Data collection top
Bruker P4 diffractometer | 1737 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.025 |
Graphite monochromator | θmax = 25.0°, θmin = 2.3° |
ω scans | h = −1→34 |
Absorption correction: ψ scan (North et al., 1968) | k = −1→11 |
Tmin = 0.625, Tmax = 0.883 | l = −10→10 |
2403 measured reflections | 3 standard reflections every 97 reflections |
1991 independent reflections | intensity decay: 1% |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0492P)2 + 7.4865P] where P = (Fo2 + 2Fc2)/3 |
1991 reflections | (Δ/σ)max = 0.023 |
175 parameters | Δρmax = 0.72 e Å−3 |
5 restraints | Δρmin = −0.49 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.35772 (2) | 0.39011 (7) | 0.97062 (7) | 0.01813 (19) | |
K2 | 0.50722 (3) | 0.23500 (9) | 0.48580 (10) | 0.0333 (2) | |
K3 | 0.24972 (2) | 0.58523 (7) | 0.68176 (7) | 0.01532 (18) | |
O1 | 0.35377 (7) | 0.3522 (2) | 0.2843 (2) | 0.0161 (4) | |
N1 | 0.33734 (8) | 0.2321 (3) | 0.3317 (3) | 0.0131 (5) | |
N2 | 0.31392 (9) | 0.1358 (3) | 0.2399 (3) | 0.0160 (5) | |
O2 | 0.30721 (8) | 0.1684 (3) | 0.0941 (2) | 0.0225 (5) | |
O3 | 0.41977 (10) | 0.1167 (3) | 0.5634 (4) | 0.0543 (10) | |
N3 | 0.39080 (9) | 0.2223 (3) | 0.5762 (3) | 0.0209 (6) | |
N4 | 0.40364 (9) | 0.3434 (3) | 0.6391 (3) | 0.0215 (6) | |
O4 | 0.44821 (8) | 0.3517 (3) | 0.6965 (3) | 0.0308 (6) | |
C1 | 0.34113 (10) | 0.2065 (3) | 0.5000 (3) | 0.0168 (6) | |
H1 | 0.3315 | 0.1048 | 0.5145 | 0.020* | |
C2 | 0.30846 (10) | 0.3065 (4) | 0.5767 (3) | 0.0182 (7) | |
O5 | 0.28639 (8) | 0.4013 (2) | 0.4934 (3) | 0.0233 (5) | |
O6 | 0.30695 (9) | 0.2768 (3) | 0.7161 (3) | 0.0333 (6) | |
O1W | 0.5000 | 0.0054 (4) | 0.2500 | 0.0395 (9) | |
H1W | 0.4743 (9) | −0.034 (5) | 0.219 (5) | 0.047* | |
O2W | 0.59716 (10) | 0.1356 (3) | 0.5823 (3) | 0.0365 (6) | |
H2W | 0.5957 (16) | 0.057 (2) | 0.537 (5) | 0.044* | |
H3W | 0.6201 (10) | 0.122 (5) | 0.653 (4) | 0.044* | |
O3W | 0.44623 (9) | 0.3590 (3) | 0.2423 (4) | 0.0357 (6) | |
H4W | 0.4491 (16) | 0.4462 (14) | 0.231 (5) | 0.043* | |
H5W | 0.4194 (7) | 0.344 (5) | 0.259 (5) | 0.043* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0180 (3) | 0.0193 (4) | 0.0168 (3) | −0.0003 (3) | 0.0024 (2) | 0.0001 (2) |
K2 | 0.0252 (4) | 0.0345 (5) | 0.0405 (5) | 0.0037 (3) | 0.0071 (3) | −0.0011 (4) |
K3 | 0.0145 (3) | 0.0160 (3) | 0.0161 (3) | 0.0003 (2) | 0.0047 (2) | −0.0012 (2) |
O1 | 0.0178 (10) | 0.0141 (10) | 0.0177 (10) | −0.0035 (8) | 0.0064 (8) | 0.0022 (8) |
N1 | 0.0141 (12) | 0.0108 (12) | 0.0145 (12) | −0.0003 (10) | 0.0030 (9) | 0.0005 (9) |
N2 | 0.0152 (12) | 0.0182 (13) | 0.0148 (12) | −0.0017 (10) | 0.0033 (9) | −0.0031 (10) |
O2 | 0.0256 (12) | 0.0277 (13) | 0.0132 (11) | −0.0051 (10) | 0.0015 (8) | −0.0010 (9) |
O3 | 0.0421 (17) | 0.0245 (15) | 0.079 (2) | 0.0209 (13) | −0.0340 (15) | −0.0238 (14) |
N3 | 0.0229 (14) | 0.0141 (13) | 0.0218 (13) | 0.0040 (11) | −0.0058 (11) | 0.0001 (10) |
N4 | 0.0163 (13) | 0.0194 (14) | 0.0269 (14) | 0.0004 (11) | −0.0008 (10) | −0.0039 (11) |
O4 | 0.0164 (11) | 0.0295 (13) | 0.0415 (14) | 0.0026 (10) | −0.0080 (10) | −0.0077 (11) |
C1 | 0.0208 (15) | 0.0134 (14) | 0.0147 (14) | −0.0043 (12) | −0.0004 (11) | 0.0008 (11) |
C2 | 0.0186 (16) | 0.0237 (16) | 0.0136 (14) | −0.0127 (13) | 0.0063 (12) | −0.0067 (13) |
O5 | 0.0225 (12) | 0.0251 (12) | 0.0239 (11) | −0.0005 (10) | 0.0083 (9) | −0.0075 (10) |
O6 | 0.0360 (14) | 0.0503 (17) | 0.0155 (11) | −0.0272 (12) | 0.0094 (10) | −0.0048 (11) |
O1W | 0.030 (2) | 0.037 (2) | 0.047 (2) | 0.000 | −0.0037 (17) | 0.000 |
O2W | 0.0440 (16) | 0.0248 (14) | 0.0396 (16) | 0.0001 (12) | 0.0052 (12) | −0.0062 (12) |
O3W | 0.0247 (13) | 0.0260 (13) | 0.0591 (17) | 0.0040 (12) | 0.0149 (12) | 0.0067 (13) |
Geometric parameters (Å, º) top
K1—O6 | 2.628 (2) | N1—N2 | 1.301 (3) |
K1—O1i | 2.758 (2) | N1—C1 | 1.458 (4) |
K1—O2Wii | 2.780 (3) | N1—K3x | 3.122 (2) |
K1—O2i | 2.845 (2) | N2—O2 | 1.276 (3) |
K1—O5iii | 2.861 (2) | N2—K3viii | 2.918 (3) |
K1—O1iii | 2.880 (2) | N2—K3x | 3.174 (3) |
K1—N4iii | 3.051 (3) | O2—K3xi | 2.745 (2) |
K1—O3Wi | 3.146 (3) | O2—K1ix | 2.845 (2) |
K1—C2iii | 3.363 (3) | O2—K3x | 3.008 (2) |
K1—N4 | 3.400 (3) | O3—N3 | 1.307 (4) |
K1—K3iii | 3.8961 (10) | N3—N4 | 1.277 (4) |
K2—O2W | 2.734 (3) | N3—C1 | 1.469 (4) |
K2—O3W | 2.736 (3) | N4—O4 | 1.291 (3) |
K2—O3Wiv | 2.828 (3) | N4—K1x | 3.051 (3) |
K2—O4 | 2.922 (3) | O4—K2ii | 3.012 (3) |
K2—O1W | 2.934 (3) | C1—C2 | 1.557 (4) |
K2—O3 | 2.940 (4) | C1—H1 | 1.0000 |
K2—O4ii | 3.012 (3) | C2—O5 | 1.238 (4) |
K2—O1Wv | 3.232 (3) | C2—O6 | 1.245 (4) |
K2—K2iv | 4.0212 (18) | C2—K1x | 3.363 (3) |
K2—K1ii | 4.1044 (11) | O5—K3x | 2.709 (2) |
K3—O6vi | 2.676 (2) | O5—K1x | 2.861 (2) |
K3—O5 | 2.709 (2) | O6—K3xii | 2.676 (2) |
K3—O5iii | 2.709 (2) | O1W—K2iv | 2.934 (3) |
K3—O2vii | 2.745 (2) | O1W—K2v | 3.231 (3) |
K3—N2viii | 2.918 (3) | O1W—K2xiii | 3.232 (3) |
K3—O2iii | 3.008 (2) | O1W—H1W | 0.828 (10) |
K3—O1iii | 3.024 (2) | O2W—K1ii | 2.780 (3) |
K3—N1iii | 3.122 (2) | O2W—H2W | 0.830 (10) |
K3—N2iii | 3.174 (3) | O2W—H3W | 0.824 (10) |
K3—O6 | 3.297 (3) | O3W—K2iv | 2.828 (3) |
O1—N1 | 1.309 (3) | O3W—K1ix | 3.146 (3) |
O1—K1ix | 2.758 (2) | O3W—H4W | 0.824 (10) |
O1—K1x | 2.880 (2) | O3W—H5W | 0.825 (10) |
O1—K3x | 3.024 (2) | | |
| | | |
O6—K1—O1i | 130.86 (7) | O6vi—K3—O1iii | 114.09 (7) |
O6—K1—O2Wii | 74.07 (9) | O5—K3—O1iii | 79.73 (6) |
O1i—K1—O2Wii | 99.10 (7) | O5iii—K3—O1iii | 61.03 (6) |
O6—K1—O2i | 77.21 (7) | O2vii—K3—O1iii | 127.02 (6) |
O1i—K1—O2i | 54.64 (6) | N2viii—K3—O1iii | 134.43 (7) |
O2Wii—K1—O2i | 74.41 (8) | O2iii—K3—O1iii | 50.49 (6) |
O6—K1—O5iii | 91.93 (8) | O6vi—K3—N1iii | 89.81 (8) |
O1i—K1—O5iii | 81.87 (6) | O5—K3—N1iii | 102.60 (7) |
O2Wii—K1—O5iii | 162.43 (8) | O5iii—K3—N1iii | 54.86 (6) |
O2i—K1—O5iii | 92.42 (7) | O2vii—K3—N1iii | 121.04 (7) |
O6—K1—O1iii | 84.69 (7) | N2viii—K3—N1iii | 141.52 (7) |
O1i—K1—O1iii | 130.71 (5) | O2iii—K3—N1iii | 41.23 (6) |
O2Wii—K1—O1iii | 126.07 (7) | O1iii—K3—N1iii | 24.53 (6) |
O2i—K1—O1iii | 147.57 (7) | O6vi—K3—N2iii | 77.10 (8) |
O5iii—K1—O1iii | 61.23 (6) | O5—K3—N2iii | 109.34 (7) |
O6—K1—N4iii | 148.35 (8) | O5iii—K3—N2iii | 72.28 (6) |
O1i—K1—N4iii | 74.20 (7) | O2vii—K3—N2iii | 98.32 (7) |
O2Wii—K1—N4iii | 126.57 (8) | N2viii—K3—N2iii | 155.93 (4) |
O2i—K1—N4iii | 128.13 (7) | O2iii—K3—N2iii | 23.62 (6) |
O5iii—K1—N4iii | 70.72 (7) | O1iii—K3—N2iii | 43.78 (6) |
O1iii—K1—N4iii | 63.84 (7) | N1iii—K3—N2iii | 23.82 (6) |
O6—K1—O3Wi | 146.88 (8) | O6vi—K3—O6 | 151.19 (5) |
O1i—K1—O3Wi | 55.19 (7) | O5—K3—O6 | 42.22 (6) |
O2Wii—K1—O3Wi | 72.83 (8) | O5iii—K3—O6 | 81.61 (6) |
O2i—K1—O3Wi | 93.09 (7) | O2vii—K3—O6 | 122.18 (6) |
O5iii—K1—O3Wi | 120.36 (7) | N2viii—K3—O6 | 72.00 (6) |
O1iii—K1—O3Wi | 115.92 (7) | O2iii—K3—O6 | 113.36 (6) |
N4iii—K1—O3Wi | 59.86 (7) | O1iii—K3—O6 | 71.84 (6) |
O6—K1—C2iii | 111.55 (8) | N1iii—K3—O6 | 94.80 (6) |
O1i—K1—C2iii | 75.12 (7) | N2iii—K3—O6 | 115.49 (6) |
O2Wii—K1—C2iii | 173.69 (8) | O6vi—K3—C2 | 170.29 (8) |
O2i—K1—C2iii | 103.62 (7) | O5—K3—C2 | 20.74 (7) |
O5iii—K1—C2iii | 21.02 (7) | O5iii—K3—C2 | 100.58 (7) |
O1iii—K1—C2iii | 58.56 (6) | O2vii—K3—C2 | 103.66 (7) |
N4iii—K1—C2iii | 49.87 (7) | N2viii—K3—C2 | 83.51 (7) |
O3Wi—K1—C2iii | 101.47 (7) | O2iii—K3—C2 | 101.20 (7) |
O6—K1—N4 | 59.08 (7) | O1iii—K3—C2 | 72.64 (6) |
O1i—K1—N4 | 154.94 (7) | N1iii—K3—C2 | 97.16 (7) |
O2Wii—K1—N4 | 59.05 (8) | N2iii—K3—C2 | 111.76 (7) |
O2i—K1—N4 | 121.99 (7) | O6—K3—C2 | 21.71 (7) |
O5iii—K1—N4 | 122.78 (7) | O6vi—K3—K1x | 134.83 (6) |
O1iii—K1—N4 | 67.42 (6) | O5—K3—K1x | 47.24 (5) |
N4iii—K1—N4 | 107.70 (7) | O5iii—K3—K1x | 105.33 (5) |
O3Wi—K1—N4 | 103.25 (7) | O2vii—K3—K1x | 88.72 (5) |
C2iii—K1—N4 | 125.94 (7) | N2viii—K3—K1x | 137.85 (5) |
O6—K1—C2 | 16.29 (7) | O2iii—K3—K1x | 46.50 (4) |
O1i—K1—C2 | 147.05 (7) | O1iii—K3—K1x | 44.81 (4) |
O2Wii—K1—C2 | 76.73 (8) | N1iii—K3—K1x | 60.46 (5) |
O2i—K1—C2 | 93.42 (7) | N2iii—K3—K1x | 62.15 (5) |
O5iii—K1—C2 | 92.85 (7) | O6—K3—K1x | 70.33 (4) |
O1iii—K1—C2 | 71.10 (7) | C2—K3—K1x | 54.88 (5) |
N4iii—K1—C2 | 134.59 (8) | N1—O1—K1ix | 120.03 (16) |
O3Wi—K1—C2 | 145.81 (7) | N1—O1—K1x | 120.99 (15) |
C2iii—K1—C2 | 109.48 (9) | K1ix—O1—K1x | 116.04 (7) |
N4—K1—C2 | 46.18 (6) | N1—O1—K3x | 81.92 (14) |
O6—K1—K3iii | 92.65 (6) | K1ix—O1—K3x | 84.60 (6) |
O1i—K1—K3iii | 50.59 (5) | K1x—O1—K3x | 86.45 (6) |
O2Wii—K1—K3iii | 124.47 (6) | N2—N1—O1 | 125.0 (2) |
O2i—K1—K3iii | 50.07 (5) | N2—N1—C1 | 115.6 (2) |
O5iii—K1—K3iii | 44.03 (4) | O1—N1—C1 | 119.2 (2) |
O1iii—K1—K3iii | 105.11 (4) | N2—N1—K3x | 80.35 (15) |
N4iii—K1—K3iii | 92.43 (5) | O1—N1—K3x | 73.55 (13) |
O3Wi—K1—K3iii | 105.30 (5) | C1—N1—K3x | 114.16 (17) |
C2iii—K1—K3iii | 53.74 (5) | O2—N2—N1 | 114.0 (2) |
N4—K1—K3iii | 150.68 (5) | O2—N2—K3viii | 114.18 (17) |
C2—K1—K3iii | 104.56 (5) | N1—N2—K3viii | 128.44 (17) |
O2W—K2—O3W | 144.67 (9) | O2—N2—K3x | 70.85 (15) |
O2W—K2—O3Wiv | 78.77 (9) | N1—N2—K3x | 75.83 (15) |
O3W—K2—O3Wiv | 67.16 (10) | K3viii—N2—K3x | 103.89 (7) |
O2W—K2—O4 | 124.34 (8) | N2—O2—K3xi | 138.48 (18) |
O3W—K2—O4 | 87.56 (8) | N2—O2—K1ix | 123.25 (17) |
O3Wiv—K2—O4 | 133.54 (8) | K3xi—O2—K1ix | 98.27 (7) |
O2W—K2—O1W | 84.68 (6) | N2—O2—K3x | 85.53 (15) |
O3W—K2—O1W | 79.60 (8) | K3xi—O2—K3x | 99.49 (7) |
O3Wiv—K2—O1W | 78.14 (7) | K1ix—O2—K3x | 83.43 (7) |
O4—K2—O1W | 136.82 (6) | N3—O3—K2 | 109.0 (2) |
O2W—K2—O3 | 127.50 (9) | N4—N3—O3 | 124.1 (3) |
O3W—K2—O3 | 82.94 (8) | N4—N3—C1 | 117.5 (2) |
O3Wiv—K2—O3 | 148.13 (9) | O3—N3—C1 | 118.2 (3) |
O4—K2—O3 | 51.26 (7) | N3—N4—O4 | 114.0 (3) |
O1W—K2—O3 | 86.11 (7) | N3—N4—K1x | 116.64 (18) |
O2W—K2—O4ii | 67.85 (8) | O4—N4—K1x | 116.63 (19) |
O3W—K2—O4ii | 130.91 (8) | N3—N4—K1 | 110.15 (19) |
O3Wiv—K2—O4ii | 108.13 (8) | O4—N4—K1 | 100.54 (18) |
O4—K2—O4ii | 59.79 (8) | K1x—N4—K1 | 95.53 (7) |
O1W—K2—O4ii | 149.30 (7) | N4—O4—K2 | 113.00 (18) |
O3—K2—O4ii | 99.57 (8) | N4—O4—K2ii | 123.8 (2) |
O2W—K2—O1Wv | 74.42 (6) | K2—O4—K2ii | 103.59 (8) |
O3W—K2—O1Wv | 136.02 (6) | N1—C1—N3 | 108.6 (2) |
O3Wiv—K2—O1Wv | 151.18 (7) | N1—C1—C2 | 112.8 (2) |
O4—K2—O1Wv | 72.29 (7) | N3—C1—C2 | 111.4 (2) |
O1W—K2—O1Wv | 88.93 (2) | N1—C1—H1 | 108.0 |
O3—K2—O1Wv | 53.81 (6) | N3—C1—H1 | 108.0 |
O4ii—K2—O1Wv | 71.18 (7) | C2—C1—H1 | 108.0 |
O2W—K2—K2iv | 102.95 (7) | O5—C2—O6 | 128.0 (3) |
O3W—K2—K2iv | 44.64 (6) | O5—C2—C1 | 117.7 (2) |
O3Wiv—K2—K2iv | 42.83 (6) | O6—C2—C1 | 114.3 (3) |
O4—K2—K2iv | 131.98 (6) | O5—C2—K3 | 50.83 (15) |
O1W—K2—K2iv | 46.74 (6) | O6—C2—K3 | 78.3 (2) |
O3—K2—K2iv | 107.39 (7) | C1—C2—K3 | 164.7 (2) |
O4ii—K2—K2iv | 150.63 (5) | O5—C2—K1x | 56.01 (15) |
O1Wv—K2—K2iv | 135.12 (5) | O6—C2—K1x | 122.9 (2) |
O2W—K2—K1ii | 42.33 (6) | C1—C2—K1x | 93.83 (16) |
O3W—K2—K1ii | 112.72 (6) | K3—C2—K1x | 71.38 (7) |
O3Wiv—K2—K1ii | 49.93 (6) | O5—C2—K1 | 118.5 (2) |
O4—K2—K1ii | 117.63 (5) | O6—C2—K1 | 36.30 (14) |
O1W—K2—K1ii | 105.32 (3) | C1—C2—K1 | 112.07 (17) |
O3—K2—K1ii | 161.76 (7) | K3—C2—K1 | 72.41 (6) |
O4ii—K2—K1ii | 63.37 (5) | K1x—C2—K1 | 87.89 (7) |
O1Wv—K2—K1ii | 111.25 (2) | C2—O5—K3 | 108.42 (18) |
K2iv—K2—K1ii | 90.68 (3) | C2—O5—K3x | 132.54 (19) |
O2W—K2—H2W | 15.7 (4) | K3—O5—K3x | 116.40 (8) |
O3W—K2—H2W | 138.9 (8) | C2—O5—K1x | 102.97 (18) |
O3Wiv—K2—H2W | 80.2 (9) | K3—O5—K1x | 88.73 (7) |
O4—K2—H2W | 133.6 (8) | K3x—O5—K1x | 93.08 (7) |
O1W—K2—H2W | 69.5 (5) | C2—O6—K1 | 127.41 (19) |
O3—K2—H2W | 120.0 (8) | C2—O6—K3xii | 126.90 (19) |
O4ii—K2—H2W | 81.8 (5) | K1—O6—K3xii | 105.69 (8) |
O1Wv—K2—H2W | 71.2 (9) | C2—O6—K3 | 79.9 (2) |
K2iv—K2—H2W | 94.3 (8) | K1—O6—K3 | 85.29 (7) |
K1ii—K2—H2W | 54.3 (6) | K3xii—O6—K3 | 106.48 (8) |
O2W—K2—H5W | 158.3 (6) | K2—O1W—K2iv | 86.52 (12) |
O3W—K2—H5W | 14.9 (5) | K2—O1W—K2v | 91.07 (2) |
O3Wiv—K2—H5W | 82.1 (5) | K2iv—O1W—K2v | 171.82 (5) |
O4—K2—H5W | 76.6 (7) | K2—O1W—K2xiii | 171.82 (5) |
O1W—K2—H5W | 81.6 (9) | K2iv—O1W—K2xiii | 91.07 (2) |
O3—K2—H5W | 68.2 (5) | K2v—O1W—K2xiii | 92.36 (11) |
O4ii—K2—H5W | 128.6 (9) | K2—O1W—H1W | 120 (3) |
O1Wv—K2—H5W | 121.8 (5) | K2iv—O1W—H1W | 99 (3) |
K2iv—K2—H5W | 55.6 (6) | K2v—O1W—H1W | 75 (3) |
K1ii—K2—H5W | 126.7 (6) | K2xiii—O1W—H1W | 68 (3) |
H2W—K2—H5W | 148.5 (10) | K2—O2W—K1ii | 96.19 (9) |
O6vi—K3—O5 | 161.70 (7) | K2—O2W—H2W | 101 (3) |
O6vi—K3—O5iii | 77.92 (7) | K1ii—O2W—H2W | 131 (3) |
O5—K3—O5iii | 120.22 (7) | K2—O2W—H3W | 150 (3) |
O6vi—K3—O2vii | 78.20 (7) | K1ii—O2W—H3W | 85 (3) |
O5—K3—O2vii | 83.85 (7) | H2W—O2W—H3W | 101 (5) |
O5iii—K3—O2vii | 155.77 (7) | K2—O3W—K2iv | 92.53 (8) |
O6vi—K3—N2viii | 86.82 (8) | K2—O3W—K1ix | 158.52 (10) |
O5—K3—N2viii | 91.49 (7) | K2iv—O3W—K1ix | 86.61 (8) |
O5iii—K3—N2viii | 87.04 (7) | K2—O3W—H4W | 116 (3) |
O2vii—K3—N2viii | 95.72 (7) | K2iv—O3W—H4W | 104 (3) |
O6vi—K3—O2iii | 88.50 (8) | K1ix—O3W—H4W | 85 (3) |
O5—K3—O2iii | 92.06 (7) | K2—O3W—H5W | 107 (3) |
O5iii—K3—O2iii | 94.77 (6) | K2iv—O3W—H5W | 130 (3) |
O2vii—K3—O2iii | 80.51 (7) | K1ix—O3W—H5W | 59 (3) |
N2viii—K3—O2iii | 174.52 (7) | H4W—O3W—H5W | 108 (5) |
| | | |
O1—N1—N2—O2 | −0.8 (4) | O3—N3—N4—O4 | −2.9 (5) |
Symmetry codes: (i) x, y, z+1; (ii) −x+1, y, −z+3/2; (iii) x, −y+1, z+1/2; (iv) −x+1, y, −z+1/2; (v) −x+1, −y, −z+1; (vi) −x+1/2, y+1/2, −z+3/2; (vii) −x+1/2, y+1/2, −z+1/2; (viii) −x+1/2, −y+1/2, −z+1; (ix) x, y, z−1; (x) x, −y+1, z−1/2; (xi) −x+1/2, y−1/2, −z+1/2; (xii) −x+1/2, y−1/2, −z+3/2; (xiii) x, −y, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O3xiii | 0.83 (1) | 2.02 (2) | 2.805 (3) | 158 (5) |
O2W—H2W···O3v | 0.83 (1) | 1.85 (1) | 2.667 (4) | 169 (5) |
O3W—H4W···O4x | 0.82 (1) | 1.90 (1) | 2.723 (4) | 174 (5) |
O3W—H5W···O1 | 0.83 (1) | 1.95 (2) | 2.757 (3) | 168 (5) |
Symmetry codes: (v) −x+1, −y, −z+1; (x) x, −y+1, z−1/2; (xiii) x, −y, z−1/2. |