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The title compound, 2Na+·C4H8N4O52-·1.5H2O, contains a 4-hydroxybutane-1,1-diylbis(diazeniumdiolate) anion with two planar diazeniumdiolate substituents. The dihedral angle between the mean planes passing through the substituents is 57.52 (7)°.
Supporting information
CCDC reference: 271879
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.002 Å
- H-atom completeness 73%
- Disorder in main residue
- R factor = 0.029
- wR factor = 0.074
- Data-to-parameter ratio = 8.7
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
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.99 <> 1.01
From the CIF: _cell_formula_units_Z 8
From the CIF: _chemical_formula_weight 265.15
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 4.00 48.04
H 1.01 8.00 8.06
N 14.01 4.00 56.03
O 16.00 6.49 103.91
Na 22.99 2.01 46.09
Calculated formula weight 262.14
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 265.15
PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.67
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.67 Ratio
PLAT301_ALERT_3_C Main Residue Disorder ......................... 11.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O2W
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O2WA
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O1W
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.77 Ratio
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C4 H11 N4 Na2 O6.5
Atom count from the _atom_site data: C4 H8 N4 Na2.005 O6.495
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 8
From the CIF: _chemical_formula_sum C4 H11 N4 Na2 O6.50
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 32.00 32.00 0.00
H 88.00 64.00 24.00
N 32.00 32.00 0.00
Na 16.00 16.04 -0.04
O 52.00 51.96 0.04
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
2 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.
Disodium 4-hydroxybutane-1,1-diylbis(diazeniumdiolate) sesquihydrate
top
Crystal data top
2Na+·C4H8N4O52−·1.5H2O | F(000) = 1096 |
Mr = 265.15 | Dx = 1.738 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 34 reflections |
a = 15.2039 (13) Å | θ = 5.0–12.5° |
b = 7.0727 (6) Å | µ = 0.23 mm−1 |
c = 19.4242 (19) Å | T = 298 K |
β = 104.018 (12)° | Prism, colorless |
V = 2026.5 (3) Å3 | 0.54 × 0.40 × 0.30 mm |
Z = 8 | |
Data collection top
Bruker P4 diffractometer | 1664 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.015 |
Graphite monochromator | θmax = 25.0°, θmin = 3.3° |
ω scans | h = −17→17 |
Absorption correction: ψ scan (SHELXS97; Sheldrick, 1997) | k = −8→1 |
Tmin = 0.882, Tmax = 0.930 | l = −23→23 |
4119 measured reflections | 3 standard reflections every 97 reflections |
1761 independent reflections | intensity decay: 1% |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.029 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.074 | w = 1/[σ2(Fo2) + (0.0325P)2 + 1.8675P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max = 0.001 |
1761 reflections | Δρmax = 0.28 e Å−3 |
203 parameters | Δρmin = −0.16 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0121 (8) |
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 | Occ. (<1) |
Na1 | 0.78714 (4) | 0.74127 (8) | 0.72948 (3) | 0.02653 (19) | |
Na2 | 0.5000 | 0.94087 (12) | 0.2500 | 0.0307 (2) | |
Na3 | 0.62581 (11) | 0.99133 (19) | 0.62045 (13) | 0.0365 (8) | 0.505 (6) |
O1 | 0.71689 (7) | 0.42613 (15) | 0.31065 (6) | 0.0324 (3) | |
N1 | 0.64553 (8) | 0.34608 (17) | 0.32341 (6) | 0.0232 (3) | |
N2 | 0.61141 (9) | 0.18831 (19) | 0.29638 (7) | 0.0294 (3) | |
O2 | 0.65300 (8) | 0.11157 (16) | 0.25345 (6) | 0.0359 (3) | |
O3 | 0.59725 (7) | 0.75192 (14) | 0.34453 (6) | 0.0288 (3) | |
N3 | 0.55339 (8) | 0.59882 (17) | 0.35128 (6) | 0.0218 (3) | |
N4 | 0.46628 (8) | 0.58718 (18) | 0.34016 (6) | 0.0263 (3) | |
O4 | 0.42438 (7) | 0.74266 (16) | 0.31987 (6) | 0.0327 (3) | |
C1 | 0.60249 (10) | 0.4241 (2) | 0.37739 (7) | 0.0224 (3) | |
H1 | 0.5570 (11) | 0.338 (2) | 0.3830 (8) | 0.018 (4)* | |
C2 | 0.67243 (11) | 0.4583 (2) | 0.44645 (8) | 0.0302 (4) | |
H2A | 0.7019 (14) | 0.337 (3) | 0.4616 (11) | 0.044 (5)* | |
H2B | 0.7169 (14) | 0.549 (3) | 0.4393 (10) | 0.042 (5)* | |
C3 | 0.63036 (12) | 0.5282 (3) | 0.50474 (8) | 0.0351 (4) | |
H3A | 0.5814 (14) | 0.442 (3) | 0.5114 (11) | 0.046 (5)* | |
H3B | 0.6040 (14) | 0.651 (3) | 0.4912 (11) | 0.047 (6)* | |
C4 | 0.70028 (12) | 0.5451 (3) | 0.57429 (9) | 0.0372 (4) | |
H4A | 0.7538 (15) | 0.609 (3) | 0.5671 (11) | 0.045 (5)* | |
H4B | 0.7177 (16) | 0.413 (4) | 0.5916 (13) | 0.066 (7)* | |
O5 | 0.67049 (8) | 0.65524 (17) | 0.62542 (6) | 0.0342 (3) | |
H5 | 0.6299 (17) | 0.596 (3) | 0.6351 (13) | 0.061 (7)* | |
O1W | 0.5896 (3) | 0.9930 (5) | 0.5771 (3) | 0.0653 (11) | 0.495 (6) |
O2W | 0.53429 (17) | 1.0307 (4) | 0.42882 (13) | 0.0442 (9) | 0.532 (5) |
O2WA | 0.6002 (2) | 1.0201 (5) | 0.4780 (2) | 0.0681 (14) | 0.468 (5) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0224 (3) | 0.0310 (3) | 0.0260 (3) | −0.0024 (2) | 0.0055 (2) | 0.0003 (2) |
Na2 | 0.0256 (4) | 0.0228 (4) | 0.0405 (5) | 0.000 | 0.0020 (3) | 0.000 |
Na3 | 0.0291 (9) | 0.0339 (8) | 0.0455 (15) | 0.0023 (6) | 0.0071 (8) | −0.0022 (6) |
O1 | 0.0320 (6) | 0.0270 (6) | 0.0460 (6) | −0.0077 (5) | 0.0247 (5) | −0.0060 (5) |
N1 | 0.0228 (6) | 0.0209 (6) | 0.0279 (6) | −0.0011 (5) | 0.0098 (5) | 0.0009 (5) |
N2 | 0.0305 (7) | 0.0266 (7) | 0.0330 (7) | −0.0033 (5) | 0.0112 (5) | −0.0055 (5) |
O2 | 0.0430 (7) | 0.0295 (6) | 0.0413 (6) | −0.0062 (5) | 0.0221 (5) | −0.0124 (5) |
O3 | 0.0265 (5) | 0.0214 (5) | 0.0388 (6) | −0.0020 (4) | 0.0083 (4) | 0.0034 (4) |
N3 | 0.0214 (6) | 0.0219 (6) | 0.0224 (6) | −0.0003 (5) | 0.0059 (4) | 0.0006 (5) |
N4 | 0.0236 (6) | 0.0287 (7) | 0.0267 (6) | 0.0014 (5) | 0.0065 (5) | 0.0009 (5) |
O4 | 0.0243 (5) | 0.0342 (6) | 0.0375 (6) | 0.0087 (5) | 0.0035 (4) | 0.0033 (5) |
C1 | 0.0236 (7) | 0.0210 (7) | 0.0246 (7) | 0.0015 (6) | 0.0098 (6) | 0.0016 (6) |
C2 | 0.0269 (8) | 0.0347 (9) | 0.0278 (8) | 0.0075 (7) | 0.0046 (6) | 0.0027 (7) |
C3 | 0.0341 (9) | 0.0432 (10) | 0.0266 (8) | 0.0040 (8) | 0.0045 (7) | −0.0044 (7) |
C4 | 0.0351 (9) | 0.0465 (11) | 0.0289 (8) | 0.0026 (8) | 0.0052 (7) | −0.0053 (7) |
O5 | 0.0377 (7) | 0.0399 (7) | 0.0264 (6) | −0.0091 (5) | 0.0105 (5) | −0.0076 (5) |
O1W | 0.083 (3) | 0.066 (2) | 0.039 (2) | 0.0272 (19) | 0.000 (2) | −0.0100 (16) |
O2W | 0.0481 (17) | 0.0417 (14) | 0.0422 (15) | 0.0044 (11) | 0.0095 (12) | 0.0006 (11) |
O2WA | 0.058 (2) | 0.067 (2) | 0.084 (3) | −0.0001 (18) | 0.027 (2) | 0.0133 (19) |
Geometric parameters (Å, º) top
Na1—O4i | 2.3822 (12) | O1—N1 | 1.2997 (15) |
Na1—O1ii | 2.4176 (12) | O1—Na1xiii | 2.4176 (12) |
Na1—O5 | 2.4216 (13) | O1—Na1iii | 2.4742 (13) |
Na1—O2ii | 2.4330 (13) | O1—Na3iii | 2.510 (2) |
Na1—O1iii | 2.4742 (13) | N1—N2 | 1.2876 (18) |
Na1—O3iii | 2.5264 (12) | N1—C1 | 1.4712 (18) |
Na1—O2iv | 2.6496 (13) | N2—O2 | 1.2826 (17) |
Na1—Na3 | 3.334 (2) | N2—Na2xiv | 2.4503 (14) |
Na1—Na3v | 3.392 (2) | O2—Na1xiii | 2.4331 (13) |
Na1—Na2iii | 3.4158 (7) | O2—Na2xiv | 2.6072 (12) |
Na1—Na1vi | 3.8539 (5) | O2—Na3xiii | 2.619 (3) |
Na1—Na1v | 3.8539 (5) | O2—Na1iv | 2.6496 (13) |
Na2—O4 | 2.4259 (12) | O3—N3 | 1.2948 (16) |
Na2—O4vii | 2.4259 (12) | O3—Na1iii | 2.5264 (12) |
Na2—N2viii | 2.4503 (14) | N3—N4 | 1.2920 (17) |
Na2—N2ix | 2.4503 (14) | N3—C1 | 1.4691 (18) |
Na2—O3vii | 2.4553 (11) | N4—O4 | 1.2840 (17) |
Na2—O3 | 2.4553 (11) | O4—Na1x | 2.3822 (12) |
Na2—O2viii | 2.6072 (12) | O4—Na3xi | 2.4277 (18) |
Na2—O2ix | 2.6072 (12) | C1—C2 | 1.516 (2) |
Na2—Na1x | 3.4157 (7) | C1—H1 | 0.948 (17) |
Na2—Na1iii | 3.4158 (7) | C2—C3 | 1.512 (2) |
Na2—Na3xi | 3.5428 (17) | C2—H2A | 0.98 (2) |
Na2—Na3xii | 3.5429 (17) | C2—H2B | 0.96 (2) |
Na3—O2Wxi | 2.395 (3) | C3—C4 | 1.508 (2) |
Na3—O4xi | 2.4278 (18) | C3—H3A | 1.00 (2) |
Na3—O5 | 2.4678 (18) | C3—H3B | 0.97 (2) |
Na3—O1iii | 2.510 (2) | C4—O5 | 1.420 (2) |
Na3—O2ii | 2.619 (3) | C4—H4A | 0.97 (2) |
Na3—O2WA | 2.706 (5) | C4—H4B | 1.00 (3) |
Na3—Na1vi | 3.392 (2) | O5—H5 | 0.81 (3) |
Na3—Na2xi | 3.5429 (17) | | |
| | | |
O4i—Na1—O1ii | 89.38 (4) | O2viii—Na2—Na3xi | 47.45 (4) |
O4i—Na1—O5 | 163.91 (5) | O2ix—Na2—Na3xi | 123.43 (4) |
O1ii—Na1—O5 | 94.10 (5) | Na1x—Na2—Na3xi | 58.31 (3) |
O4i—Na1—O2ii | 117.63 (5) | Na1iii—Na2—Na3xi | 128.86 (4) |
O1ii—Na1—O2ii | 63.99 (4) | O4—Na2—Na3xii | 152.39 (5) |
O5—Na1—O2ii | 77.81 (4) | O4vii—Na2—Na3xii | 43.14 (3) |
O4i—Na1—O1iii | 97.89 (4) | N2viii—Na2—Na3xii | 94.95 (4) |
O1ii—Na1—O1iii | 133.63 (4) | N2ix—Na2—Na3xii | 73.76 (4) |
O5—Na1—O1iii | 91.07 (4) | O3vii—Na2—Na3xii | 82.73 (4) |
O2ii—Na1—O1iii | 72.28 (4) | O3—Na2—Na3xii | 105.90 (4) |
O4i—Na1—O3iii | 79.19 (4) | O2viii—Na2—Na3xii | 123.43 (4) |
O1ii—Na1—O3iii | 149.16 (4) | O2ix—Na2—Na3xii | 47.45 (4) |
O5—Na1—O3iii | 89.98 (4) | Na1x—Na2—Na3xii | 128.86 (4) |
O2ii—Na1—O3iii | 146.28 (4) | Na1iii—Na2—Na3xii | 58.31 (3) |
O1iii—Na1—O3iii | 76.71 (4) | Na3xi—Na2—Na3xii | 164.44 (5) |
O4i—Na1—O2iv | 74.91 (4) | O2Wxi—Na3—O4xi | 80.48 (8) |
O1ii—Na1—O2iv | 69.50 (4) | O2Wxi—Na3—O5 | 101.34 (9) |
O5—Na1—O2iv | 91.59 (4) | O4xi—Na3—O5 | 147.48 (10) |
O2ii—Na1—O2iv | 131.11 (4) | O2Wxi—Na3—O1iii | 166.65 (10) |
O1iii—Na1—O2iv | 156.41 (4) | O4xi—Na3—O1iii | 86.23 (7) |
O3iii—Na1—O2iv | 79.86 (4) | O5—Na3—O1iii | 89.16 (7) |
O4i—Na1—Na3 | 145.21 (5) | O2Wxi—Na3—O2ii | 106.17 (8) |
O1ii—Na1—Na3 | 107.51 (4) | O4xi—Na3—O2ii | 74.76 (7) |
O5—Na1—Na3 | 47.60 (4) | O5—Na3—O2ii | 73.59 (6) |
O2ii—Na1—Na3 | 51.15 (4) | O1iii—Na3—O2ii | 68.68 (7) |
O1iii—Na1—Na3 | 48.49 (4) | O2Wxi—Na3—O2WA | 73.50 (11) |
O3iii—Na1—Na3 | 97.74 (4) | O4xi—Na3—O2WA | 116.48 (11) |
O2iv—Na1—Na3 | 139.19 (4) | O5—Na3—O2WA | 94.73 (11) |
O4i—Na1—Na3v | 45.70 (4) | O1iii—Na3—O2WA | 114.19 (9) |
O1ii—Na1—Na3v | 47.65 (4) | O2ii—Na3—O2WA | 168.13 (10) |
O5—Na1—Na3v | 129.85 (5) | O2Wxi—Na3—Na1 | 137.69 (8) |
O2ii—Na1—Na3v | 103.25 (4) | O4xi—Na3—Na1 | 112.07 (9) |
O1iii—Na1—Na3v | 137.82 (5) | O5—Na3—Na1 | 46.44 (4) |
O3iii—Na1—Na3v | 108.57 (4) | O1iii—Na3—Na1 | 47.57 (5) |
O2iv—Na1—Na3v | 49.52 (4) | O2ii—Na3—Na1 | 46.35 (4) |
Na3—Na1—Na3v | 153.69 (2) | O2WA—Na3—Na1 | 126.20 (9) |
O4i—Na1—Na2iii | 45.25 (3) | O2Wxi—Na3—Na1vi | 121.64 (8) |
O1ii—Na1—Na2iii | 107.15 (3) | O4xi—Na3—Na1vi | 44.61 (4) |
O5—Na1—Na2iii | 118.96 (4) | O5—Na3—Na1vi | 114.96 (8) |
O2ii—Na1—Na2iii | 162.45 (4) | O1iii—Na3—Na1vi | 45.38 (4) |
O1iii—Na1—Na2iii | 110.23 (3) | O2ii—Na3—Na1vi | 50.32 (5) |
O3iii—Na1—Na2iii | 45.85 (3) | O2WA—Na3—Na1vi | 140.24 (10) |
O2iv—Na1—Na2iii | 48.94 (3) | Na1—Na3—Na1vi | 69.92 (5) |
Na3—Na1—Na2iii | 143.59 (3) | O2Wxi—Na3—Na2xi | 67.75 (7) |
Na3v—Na1—Na2iii | 62.72 (3) | O4xi—Na3—Na2xi | 43.10 (4) |
O4i—Na1—Na1vi | 92.98 (3) | O5—Na3—Na2xi | 107.07 (6) |
O1ii—Na1—Na1vi | 96.69 (4) | O1iii—Na3—Na2xi | 101.45 (7) |
O5—Na1—Na1vi | 102.19 (4) | O2ii—Na3—Na2xi | 47.18 (4) |
O2ii—Na1—Na1vi | 42.83 (3) | O2WA—Na3—Na2xi | 138.35 (10) |
O1iii—Na1—Na1vi | 37.50 (2) | Na1—Na3—Na2xi | 93.52 (6) |
O3iii—Na1—Na1vi | 112.29 (3) | Na1vi—Na3—Na2xi | 58.97 (4) |
O2iv—Na1—Na1vi | 161.33 (4) | N1—O1—Na1xiii | 115.59 (8) |
Na3—Na1—Na1vi | 55.75 (3) | N1—O1—Na1iii | 121.08 (9) |
Na3v—Na1—Na1vi | 111.92 (4) | Na1xiii—O1—Na1iii | 103.96 (4) |
Na2iii—Na1—Na1vi | 129.70 (2) | N1—O1—Na3iii | 136.99 (10) |
O4i—Na1—Na1v | 98.02 (3) | Na1xiii—O1—Na3iii | 86.97 (5) |
O1ii—Na1—Na1v | 38.54 (3) | Na1iii—O1—Na3iii | 83.94 (5) |
O5—Na1—Na1v | 75.53 (3) | N2—N1—O1 | 124.91 (12) |
O2ii—Na1—Na1v | 92.97 (4) | N2—N1—C1 | 114.25 (11) |
O1iii—Na1—Na1v | 162.07 (4) | O1—N1—C1 | 120.55 (11) |
O3iii—Na1—Na1v | 114.48 (3) | O2—N2—N1 | 114.73 (12) |
O2iv—Na1—Na1v | 38.63 (3) | O2—N2—Na2xiv | 82.21 (8) |
Na3—Na1—Na1v | 114.26 (3) | N1—N2—Na2xiv | 160.60 (10) |
Na3v—Na1—Na1v | 54.33 (3) | N2—O2—Na1xiii | 120.77 (9) |
Na2iii—Na1—Na1v | 86.94 (2) | N2—O2—Na2xiv | 68.62 (7) |
Na1vi—Na1—Na1v | 133.15 (3) | Na1xiii—O2—Na2xiv | 167.74 (5) |
O4—Na2—O4vii | 109.39 (6) | N2—O2—Na3xiii | 140.72 (10) |
O4—Na2—N2viii | 103.85 (4) | Na1xiii—O2—Na3xiii | 82.49 (5) |
O4vii—Na2—N2viii | 125.89 (4) | Na2xiv—O2—Na3xiii | 85.37 (5) |
O4—Na2—N2ix | 125.89 (4) | N2—O2—Na1iv | 121.72 (9) |
O4vii—Na2—N2ix | 103.84 (4) | Na1xiii—O2—Na1iv | 98.53 (4) |
N2viii—Na2—N2ix | 88.84 (7) | Na2xiv—O2—Na1iv | 81.05 (4) |
O4—Na2—O3vii | 79.78 (4) | Na3xiii—O2—Na1iv | 80.16 (5) |
O4vii—Na2—O3vii | 63.14 (4) | N3—O3—Na2 | 107.42 (8) |
N2viii—Na2—O3vii | 82.90 (4) | N3—O3—Na1iii | 121.32 (8) |
N2ix—Na2—O3vii | 154.31 (4) | Na2—O3—Na1iii | 86.56 (4) |
O4—Na2—O3 | 63.14 (4) | N4—N3—O3 | 124.65 (12) |
O4vii—Na2—O3 | 79.78 (4) | N4—N3—C1 | 114.75 (11) |
N2viii—Na2—O3 | 154.31 (4) | O3—N3—C1 | 120.49 (11) |
N2ix—Na2—O3 | 82.90 (4) | O4—N4—N3 | 114.14 (12) |
O3vii—Na2—O3 | 114.04 (6) | N4—O4—Na1x | 123.23 (9) |
O4—Na2—O2viii | 75.00 (3) | N4—O4—Na2 | 113.55 (8) |
O4vii—Na2—O2viii | 142.57 (4) | Na1x—O4—Na2 | 90.53 (4) |
N2viii—Na2—O2viii | 29.17 (4) | N4—O4—Na3xi | 134.99 (10) |
N2ix—Na2—O2viii | 102.22 (5) | Na1x—O4—Na3xi | 89.68 (6) |
O3vii—Na2—O2viii | 82.01 (4) | Na2—O4—Na3xi | 93.76 (6) |
O3—Na2—O2viii | 130.03 (4) | N3—C1—N1 | 110.24 (11) |
O4—Na2—O2ix | 142.56 (4) | N3—C1—C2 | 111.10 (12) |
O4vii—Na2—O2ix | 75.00 (3) | N1—C1—C2 | 110.67 (12) |
N2viii—Na2—O2ix | 102.22 (5) | N3—C1—H1 | 104.8 (9) |
N2ix—Na2—O2ix | 29.17 (4) | N1—C1—H1 | 107.7 (9) |
O3vii—Na2—O2ix | 130.03 (3) | C2—C1—H1 | 112.1 (9) |
O3—Na2—O2ix | 82.01 (4) | C3—C2—C1 | 112.44 (13) |
O2viii—Na2—O2ix | 124.83 (6) | C3—C2—H2A | 107.8 (12) |
O4—Na2—Na1x | 44.22 (3) | C1—C2—H2A | 107.4 (12) |
O4vii—Na2—Na1x | 106.31 (3) | C3—C2—H2B | 109.3 (12) |
N2viii—Na2—Na1x | 71.06 (3) | C1—C2—H2B | 110.1 (11) |
N2ix—Na2—Na1x | 149.69 (4) | H2A—C2—H2B | 109.7 (16) |
O3vii—Na2—Na1x | 47.59 (3) | C4—C3—C2 | 111.25 (14) |
O3—Na2—Na1x | 105.30 (3) | C4—C3—H3A | 108.6 (12) |
O2viii—Na2—Na1x | 50.02 (3) | C2—C3—H3A | 111.3 (12) |
O2ix—Na2—Na1x | 172.68 (4) | C4—C3—H3B | 109.2 (12) |
O4—Na2—Na1iii | 106.31 (3) | C2—C3—H3B | 108.2 (12) |
O4vii—Na2—Na1iii | 44.22 (3) | H3A—C3—H3B | 108.2 (17) |
N2viii—Na2—Na1iii | 149.69 (4) | O5—C4—C3 | 113.26 (14) |
N2ix—Na2—Na1iii | 71.06 (3) | O5—C4—H4A | 105.5 (12) |
O3vii—Na2—Na1iii | 105.30 (3) | C3—C4—H4A | 110.0 (12) |
O3—Na2—Na1iii | 47.59 (3) | O5—C4—H4B | 112.2 (14) |
O2viii—Na2—Na1iii | 172.68 (4) | C3—C4—H4B | 107.3 (14) |
O2ix—Na2—Na1iii | 50.02 (3) | H4A—C4—H4B | 108.5 (18) |
Na1x—Na2—Na1iii | 135.69 (3) | C4—O5—Na1 | 115.37 (10) |
O4—Na2—Na3xi | 43.14 (3) | C4—O5—Na3 | 129.24 (12) |
O4vii—Na2—Na3xi | 152.39 (5) | Na1—O5—Na3 | 85.96 (7) |
N2viii—Na2—Na3xi | 73.76 (4) | C4—O5—H5 | 105.6 (17) |
N2ix—Na2—Na3xi | 94.95 (4) | Na1—O5—H5 | 112.6 (18) |
O3vii—Na2—Na3xi | 105.90 (4) | Na3—O5—H5 | 107.0 (17) |
O3—Na2—Na3xi | 82.73 (4) | | |
| | | |
O1—N1—N2—O2 | −0.8 (2) | O3—N3—N4—O4 | 1.34 (18) |
Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) x, −y+1, z+1/2; (iii) −x+3/2, −y+3/2, −z+1; (iv) −x+3/2, −y+1/2, −z+1; (v) −x+3/2, y−1/2, −z+3/2; (vi) −x+3/2, y+1/2, −z+3/2; (vii) −x+1, y, −z+1/2; (viii) −x+1, y+1, −z+1/2; (ix) x, y+1, z; (x) x−1/2, −y+3/2, z−1/2; (xi) −x+1, −y+2, −z+1; (xii) x, −y+2, z−1/2; (xiii) x, −y+1, z−1/2; (xiv) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···N4xv | 0.81 (3) | 2.09 (3) | 2.8956 (18) | 173 (2) |
Symmetry code: (xv) −x+1, −y+1, −z+1. |
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