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The asymmetric unit cell of the title compound, (C4H14N2)3[V10O28]·6H2O, consists of one half-decavanadate anion of Ci symmetry, three water molecules, one butane-1,4-diammonium cation in a general position and one half-butane-1,4-diammonium cation in a special position of Ci symmetry. Water molecules are located within cavities of a framework formed by the anions and cations. All molecules are connected via hydrogen bonds into a three-dimensional network.
Supporting information
CCDC reference: 621321
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.037
- wR factor = 0.090
- Data-to-parameter ratio = 15.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.837(18) ...... 2.22 su-Ra
O3W -H31W 1.555 1.555
| Author Response: CIF was generated from SHELXL without any subsequent modification of
s.u. values. SHELXL is using full covariance matrix for esd's
calculation, but validation software is using only reported su's, which
can lead to discrepancies (especially if constrained/restrained
refinement is used, because this generally leads to higher su's).
|
PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.837(18) ...... 2.22 su-Ra
O3W -H31W 1.555 1.555
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997); cell refinement: COLLECT and DENZO; data reduction: COLLECT and DENZO; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2006).
butane-1,4-diammonium decavanadate(V) hexahydrate
top
Crystal data top
(C4H14N2)3[V10O28]·6H2O | F(000) = 1340 |
Mr = 1336.01 | Dx = 2.156 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71070 Å |
a = 10.6504 (4) Å | Cell parameters from 7432 reflections |
b = 17.6351 (4) Å | θ = 1.0–27.5° |
c = 10.9644 (4) Å | µ = 2.27 mm−1 |
β = 92.0375 (16)° | T = 293 K |
V = 2058.04 (12) Å3 | Prism, orange |
Z = 2 | 0.50 × 0.13 × 0.08 mm |
Data collection top
Nonius KappaCCD κ-axis diffractometer | 4706 independent reflections |
Radiation source: fine-focus sealed tube | 3665 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω and φ scans | h = 0→13 |
Absorption correction: analytical [PLATON (Spek, 2003), analytical numeric absorption correction using
a multifaceted crystal model based on de Meulenaar & Tompa (1965)] | k = 0→22 |
Tmin = 0.698, Tmax = 0.841 | l = −14→14 |
15546 measured reflections | |
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)] = 0.037 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.090 | w = 1/[σ2(Fo2) + (0.0319P)2 + 2.7675P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.001 |
4706 reflections | Δρmax = 0.43 e Å−3 |
302 parameters | Δρmin = −0.52 e Å−3 |
9 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0010 (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 | |
N11 | −0.0914 (3) | 0.40898 (15) | 0.5146 (3) | 0.0290 (6) | |
H1A | −0.0684 | 0.3957 | 0.5905 | 0.043* | |
H1B | −0.1364 | 0.4515 | 0.5162 | 0.043* | |
H1C | −0.0232 | 0.4166 | 0.4716 | 0.043* | |
C11 | −0.1686 (3) | 0.34729 (19) | 0.4570 (3) | 0.0327 (8) | |
H11A | −0.2096 | 0.3660 | 0.3826 | 0.039* | |
H11B | −0.2332 | 0.3319 | 0.5121 | 0.039* | |
C12 | −0.0876 (3) | 0.27986 (19) | 0.4280 (3) | 0.0295 (8) | |
H12A | −0.0275 | 0.2949 | 0.3681 | 0.035* | |
H12B | −0.1404 | 0.2405 | 0.3917 | 0.035* | |
C13 | −0.0170 (4) | 0.24760 (19) | 0.5382 (3) | 0.0320 (8) | |
H13B | 0.0383 | 0.2862 | 0.5731 | 0.038* | |
H13A | −0.0765 | 0.2338 | 0.5994 | 0.038* | |
C14 | 0.0597 (3) | 0.17887 (19) | 0.5067 (3) | 0.0281 (7) | |
H14A | 0.0044 | 0.1355 | 0.4954 | 0.034* | |
H14B | 0.1007 | 0.1878 | 0.4305 | 0.034* | |
N12 | 0.1557 (3) | 0.16163 (17) | 0.6037 (3) | 0.0318 (7) | |
H2C | 0.2085 | 0.2006 | 0.6121 | 0.038* | |
H2B | 0.1982 | 0.1203 | 0.5835 | 0.038* | |
H2A | 0.1182 | 0.1537 | 0.6738 | 0.038* | |
N2 | 0.4686 (3) | 0.41834 (16) | 0.7493 (2) | 0.0266 (6) | |
H21N | 0.4078 | 0.4135 | 0.8024 | 0.040* | |
H22N | 0.5338 | 0.4423 | 0.7848 | 0.040* | |
H23N | 0.4927 | 0.3726 | 0.7250 | 0.040* | |
C21 | 0.4214 (3) | 0.46247 (19) | 0.6426 (3) | 0.0273 (8) | |
H21A | 0.3870 | 0.5102 | 0.6703 | 0.033* | |
H21B | 0.3544 | 0.4345 | 0.6007 | 0.033* | |
C22 | 0.5242 (3) | 0.47814 (19) | 0.5552 (3) | 0.0254 (7) | |
H22A | 0.5598 | 0.4305 | 0.5289 | 0.030* | |
H22B | 0.5905 | 0.5070 | 0.5967 | 0.030* | |
V1 | 0.36286 (5) | 0.10082 (3) | 0.36455 (5) | 0.01565 (13) | |
V2 | 0.53309 (5) | 0.19025 (3) | 0.55474 (5) | 0.01906 (14) | |
V3 | 0.72962 (5) | 0.05850 (3) | 0.56479 (5) | 0.01630 (14) | |
V4 | 0.64286 (5) | 0.13046 (3) | 0.31686 (5) | 0.01787 (14) | |
V5 | 0.44002 (4) | 0.03174 (3) | 0.62655 (4) | 0.01411 (13) | |
O1 | 0.2327 (2) | 0.11477 (12) | 0.2889 (2) | 0.0239 (5) | |
O2 | 0.5217 (2) | 0.27138 (12) | 0.6196 (2) | 0.0290 (5) | |
O3 | 0.7176 (2) | 0.16510 (12) | 0.2047 (2) | 0.0262 (5) | |
O4 | 0.36392 (19) | −0.01536 (11) | 0.73416 (18) | 0.0196 (5) | |
O5 | 0.37977 (19) | 0.18462 (11) | 0.45940 (19) | 0.0186 (4) | |
O6 | 0.67952 (19) | 0.15042 (11) | 0.62507 (19) | 0.0198 (5) | |
O7 | 0.8610 (2) | 0.04247 (12) | 0.6377 (2) | 0.0244 (5) | |
O8 | 0.47792 (19) | 0.12904 (11) | 0.25418 (18) | 0.0183 (4) | |
O9 | 0.6160 (2) | 0.21218 (11) | 0.41241 (19) | 0.0205 (5) | |
O10 | 0.30026 (18) | 0.04351 (11) | 0.50911 (18) | 0.0151 (4) | |
O11 | 0.44187 (19) | 0.12421 (11) | 0.67032 (18) | 0.0188 (4) | |
O12 | 0.77757 (18) | 0.09557 (11) | 0.41881 (19) | 0.0177 (4) | |
O13 | 0.60929 (18) | 0.00838 (11) | 0.67872 (18) | 0.0159 (4) | |
O14 | 0.53993 (18) | 0.06896 (10) | 0.46803 (17) | 0.0146 (4) | |
O1W | 0.8558 (3) | 0.55833 (14) | 0.5882 (2) | 0.0315 (6) | |
H11W | 0.867 (4) | 0.5405 (19) | 0.657 (2) | 0.047* | |
H12W | 0.813 (3) | 0.5979 (15) | 0.588 (3) | 0.047* | |
O2W | 0.7146 (3) | 0.68284 (14) | 0.6460 (2) | 0.0412 (7) | |
H21W | 0.749 (4) | 0.689 (2) | 0.715 (2) | 0.062* | |
H22W | 0.699 (4) | 0.7264 (15) | 0.616 (3) | 0.062* | |
O3W | 0.4579 (3) | 0.64908 (14) | 0.6780 (2) | 0.0354 (6) | |
H31W | 0.432 (3) | 0.6858 (18) | 0.636 (4) | 0.053* | |
H32W | 0.5354 (17) | 0.649 (2) | 0.682 (4) | 0.053* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
N11 | 0.0359 (17) | 0.0251 (15) | 0.0259 (15) | 0.0057 (12) | 0.0011 (13) | 0.0005 (12) |
C11 | 0.0284 (19) | 0.0325 (19) | 0.036 (2) | 0.0034 (15) | −0.0105 (16) | −0.0014 (15) |
C12 | 0.033 (2) | 0.0269 (18) | 0.0282 (19) | −0.0003 (15) | −0.0059 (15) | −0.0050 (14) |
C13 | 0.038 (2) | 0.0302 (19) | 0.0275 (19) | 0.0110 (15) | 0.0031 (16) | −0.0033 (15) |
C14 | 0.0293 (19) | 0.0318 (18) | 0.0233 (18) | 0.0053 (14) | 0.0026 (14) | −0.0048 (14) |
N12 | 0.0272 (16) | 0.0346 (17) | 0.0339 (17) | 0.0089 (12) | 0.0051 (13) | −0.0012 (13) |
N2 | 0.0197 (14) | 0.0373 (16) | 0.0228 (15) | −0.0009 (12) | 0.0006 (11) | 0.0048 (12) |
C21 | 0.0221 (17) | 0.0331 (19) | 0.0269 (18) | 0.0007 (14) | 0.0019 (14) | 0.0116 (14) |
C22 | 0.0241 (17) | 0.0276 (18) | 0.0246 (18) | 0.0003 (13) | 0.0029 (14) | 0.0024 (14) |
V1 | 0.0137 (3) | 0.0161 (3) | 0.0170 (3) | 0.00222 (19) | −0.0011 (2) | 0.00265 (19) |
V2 | 0.0208 (3) | 0.0146 (3) | 0.0218 (3) | 0.0004 (2) | 0.0010 (2) | −0.0017 (2) |
V3 | 0.0134 (3) | 0.0175 (3) | 0.0178 (3) | −0.00080 (19) | −0.0021 (2) | 0.00123 (19) |
V4 | 0.0163 (3) | 0.0187 (3) | 0.0188 (3) | 0.0003 (2) | 0.0020 (2) | 0.0033 (2) |
V5 | 0.0139 (3) | 0.0150 (3) | 0.0134 (3) | 0.00147 (18) | 0.00043 (19) | −0.00092 (18) |
O1 | 0.0187 (11) | 0.0268 (12) | 0.0260 (13) | 0.0034 (9) | −0.0035 (9) | 0.0029 (9) |
O2 | 0.0351 (14) | 0.0176 (11) | 0.0343 (14) | −0.0003 (10) | 0.0015 (11) | −0.0074 (10) |
O3 | 0.0237 (12) | 0.0294 (12) | 0.0259 (13) | 0.0007 (9) | 0.0065 (10) | 0.0079 (10) |
O4 | 0.0192 (11) | 0.0239 (11) | 0.0158 (11) | 0.0009 (9) | 0.0029 (9) | 0.0014 (9) |
O5 | 0.0176 (11) | 0.0168 (11) | 0.0214 (11) | 0.0016 (8) | 0.0006 (9) | 0.0016 (8) |
O6 | 0.0207 (11) | 0.0172 (11) | 0.0213 (12) | −0.0023 (8) | −0.0021 (9) | −0.0025 (8) |
O7 | 0.0180 (11) | 0.0277 (12) | 0.0269 (12) | −0.0003 (9) | −0.0082 (9) | 0.0025 (9) |
O8 | 0.0177 (11) | 0.0209 (11) | 0.0161 (11) | 0.0017 (8) | 0.0003 (8) | 0.0047 (8) |
O9 | 0.0206 (11) | 0.0173 (11) | 0.0236 (12) | −0.0014 (8) | 0.0008 (9) | 0.0015 (8) |
O10 | 0.0124 (10) | 0.0168 (10) | 0.0160 (10) | 0.0019 (8) | −0.0001 (8) | 0.0006 (8) |
O11 | 0.0222 (11) | 0.0168 (10) | 0.0174 (11) | 0.0013 (8) | 0.0009 (9) | −0.0038 (8) |
O12 | 0.0134 (10) | 0.0184 (11) | 0.0215 (11) | −0.0009 (8) | 0.0019 (8) | 0.0011 (8) |
O13 | 0.0166 (10) | 0.0167 (10) | 0.0143 (10) | 0.0001 (8) | −0.0015 (8) | −0.0002 (8) |
O14 | 0.0135 (10) | 0.0141 (10) | 0.0160 (10) | 0.0011 (8) | −0.0009 (8) | 0.0002 (8) |
O1W | 0.0436 (16) | 0.0306 (14) | 0.0204 (13) | 0.0098 (11) | 0.0004 (11) | 0.0018 (10) |
O2W | 0.0540 (18) | 0.0337 (15) | 0.0348 (16) | 0.0158 (13) | −0.0115 (13) | 0.0020 (12) |
O3W | 0.0418 (16) | 0.0315 (14) | 0.0330 (15) | 0.0028 (12) | 0.0020 (12) | 0.0072 (11) |
Geometric parameters (Å, º) top
N11—C11 | 1.490 (4) | V1—O13ii | 2.0080 (19) |
N11—H1A | 0.8900 | V1—O14 | 2.2377 (19) |
N11—H1B | 0.8900 | V2—O2 | 1.604 (2) |
N11—H1C | 0.8900 | V2—O5 | 1.910 (2) |
C11—C12 | 1.509 (5) | V2—O6 | 1.853 (2) |
C11—H11A | 0.9700 | V2—O9 | 1.861 (2) |
C11—H11B | 0.9700 | V2—O11 | 1.998 (2) |
C12—C13 | 1.511 (5) | V2—O14 | 2.3429 (19) |
C12—H12A | 0.9700 | V3—O6 | 1.837 (2) |
C12—H12B | 0.9700 | V3—O7 | 1.611 (2) |
C13—C14 | 1.508 (4) | V3—O10ii | 1.9939 (19) |
C13—H13B | 0.9700 | V3—O12 | 1.819 (2) |
C13—H13A | 0.9700 | V3—O13 | 2.024 (2) |
C14—N12 | 1.480 (4) | V3—O14 | 2.2558 (19) |
C14—H14A | 0.9700 | V4—O3 | 1.609 (2) |
C14—H14B | 0.9700 | V4—O4ii | 2.106 (2) |
N12—H2C | 0.8900 | V4—O8 | 1.864 (2) |
N12—H2B | 0.8900 | V4—O9 | 1.810 (2) |
N12—H2A | 0.8900 | V4—O12 | 1.890 (2) |
N2—C21 | 1.478 (4) | V4—O14 | 2.292 (2) |
N2—H21N | 0.8900 | V5—O4 | 1.675 (2) |
N2—H22N | 0.8900 | V5—O10 | 1.944 (2) |
N2—H23N | 0.8900 | V5—O11 | 1.6998 (19) |
C21—C22 | 1.507 (4) | V5—O13 | 1.917 (2) |
C21—H21A | 0.9700 | V5—O14 | 2.171 (2) |
C21—H21B | 0.9700 | V5—O14ii | 2.0713 (19) |
C22—C22i | 1.510 (6) | O1W—H11W | 0.826 (18) |
C22—H22A | 0.9700 | O1W—H12W | 0.832 (18) |
C22—H22B | 0.9700 | O2W—H21W | 0.838 (18) |
V1—O1 | 1.609 (2) | O2W—H22W | 0.852 (18) |
V1—O5 | 1.812 (2) | O3W—H31W | 0.837 (18) |
V1—O8 | 1.822 (2) | O3W—H32W | 0.826 (18) |
V1—O10 | 2.013 (2) | | |
| | | |
C11—N11—H1A | 109.5 | O12—V3—O14 | 80.30 (8) |
C11—N11—H1B | 109.5 | O6—V3—O14 | 80.23 (8) |
H1A—N11—H1B | 109.5 | O10ii—V3—O14 | 75.84 (7) |
C11—N11—H1C | 109.5 | O13—V3—O14 | 75.51 (7) |
H1A—N11—H1C | 109.5 | O7—V3—V1ii | 89.70 (8) |
H1B—N11—H1C | 109.5 | O12—V3—V1ii | 130.58 (7) |
N11—C11—C12 | 110.7 (3) | O6—V3—V1ii | 127.87 (7) |
N11—C11—H11A | 109.5 | O10ii—V3—V1ii | 39.89 (6) |
C12—C11—H11A | 109.5 | O13—V3—V1ii | 39.89 (6) |
N11—C11—H11B | 109.5 | O14—V3—V1ii | 84.49 (5) |
C12—C11—H11B | 109.5 | O7—V3—V4 | 136.97 (8) |
H11A—C11—H11B | 108.1 | O12—V3—V4 | 33.72 (6) |
C11—C12—C13 | 113.6 (3) | O6—V3—V4 | 82.72 (7) |
C11—C12—H12A | 108.9 | O10ii—V3—V4 | 88.55 (6) |
C13—C12—H12A | 108.9 | O13—V3—V4 | 122.85 (6) |
C11—C12—H12B | 108.9 | O14—V3—V4 | 47.34 (5) |
C13—C12—H12B | 108.9 | V1ii—V3—V4 | 120.23 (2) |
H12A—C12—H12B | 107.7 | O3—V4—O9 | 103.45 (11) |
C14—C13—C12 | 112.2 (3) | O3—V4—O8 | 102.06 (10) |
C14—C13—H13B | 109.2 | O9—V4—O8 | 93.31 (9) |
C12—C13—H13B | 109.2 | O3—V4—O12 | 100.93 (10) |
C14—C13—H13A | 109.2 | O9—V4—O12 | 92.81 (9) |
C12—C13—H13A | 109.2 | O8—V4—O12 | 154.09 (9) |
H13B—C13—H13A | 107.9 | O3—V4—O4ii | 100.14 (10) |
N12—C14—C13 | 111.5 (3) | O9—V4—O4ii | 156.39 (9) |
N12—C14—H14A | 109.3 | O8—V4—O4ii | 82.31 (8) |
C13—C14—H14A | 109.3 | O12—V4—O4ii | 82.04 (8) |
N12—C14—H14B | 109.3 | O3—V4—O14 | 174.06 (10) |
C13—C14—H14B | 109.3 | O9—V4—O14 | 82.46 (8) |
H14A—C14—H14B | 108.0 | O8—V4—O14 | 77.97 (8) |
C14—N12—H2C | 109.5 | O12—V4—O14 | 77.93 (8) |
C14—N12—H2B | 109.5 | O4ii—V4—O14 | 73.94 (7) |
H2C—N12—H2B | 109.5 | O3—V4—V5ii | 131.55 (8) |
C14—N12—H2A | 109.5 | O9—V4—V5ii | 124.99 (7) |
H2C—N12—H2A | 109.5 | O8—V4—V5ii | 77.74 (6) |
H2B—N12—H2A | 109.5 | O12—V4—V5ii | 78.14 (6) |
C21—N2—H21N | 109.5 | O4ii—V4—V5ii | 31.41 (6) |
C21—N2—H22N | 109.5 | O14—V4—V5ii | 42.53 (5) |
H21N—N2—H22N | 109.5 | O3—V4—V2 | 136.87 (8) |
C21—N2—H23N | 109.5 | O9—V4—V2 | 33.43 (7) |
H21N—N2—H23N | 109.5 | O8—V4—V2 | 86.31 (7) |
H22N—N2—H23N | 109.5 | O12—V4—V2 | 85.05 (6) |
N2—C21—C22 | 111.5 (3) | O4ii—V4—V2 | 122.96 (6) |
N2—C21—H21A | 109.3 | O14—V4—V2 | 49.03 (5) |
C22—C21—H21A | 109.3 | V5ii—V4—V2 | 91.565 (18) |
N2—C21—H21B | 109.3 | O3—V4—V1 | 134.45 (8) |
C22—C21—H21B | 109.3 | O9—V4—V1 | 82.15 (7) |
H21A—C21—H21B | 108.0 | O8—V4—V1 | 32.60 (6) |
C21—C22—C22i | 111.6 (3) | O12—V4—V1 | 124.17 (6) |
C21—C22—H22A | 109.3 | O4ii—V4—V1 | 81.82 (6) |
C22i—C22—H22A | 109.3 | O14—V4—V1 | 46.25 (5) |
C21—C22—H22B | 109.3 | V5ii—V4—V1 | 61.387 (16) |
C22i—C22—H22B | 109.3 | V2—V4—V1 | 61.138 (16) |
H22A—C22—H22B | 108.0 | O3—V4—V3 | 133.08 (8) |
O1—V1—O5 | 103.74 (10) | O9—V4—V3 | 82.37 (7) |
O1—V1—O8 | 101.72 (10) | O8—V4—V3 | 124.31 (6) |
O5—V1—O8 | 95.91 (9) | O12—V4—V3 | 32.29 (6) |
O1—V1—O13ii | 99.01 (10) | O4ii—V4—V3 | 81.10 (6) |
O5—V1—O13ii | 154.84 (9) | O14—V4—V3 | 46.36 (5) |
O8—V1—O13ii | 89.80 (9) | V5ii—V4—V3 | 61.368 (16) |
O1—V1—O10 | 100.34 (10) | V2—V4—V3 | 60.647 (16) |
O5—V1—O10 | 89.22 (9) | V1—V4—V3 | 92.385 (19) |
O8—V1—O10 | 155.43 (9) | O4—V5—O11 | 106.13 (10) |
O13ii—V1—O10 | 76.13 (8) | O4—V5—O13 | 99.02 (9) |
O1—V1—O14 | 174.25 (9) | O11—V5—O13 | 96.92 (9) |
O5—V1—O14 | 81.32 (8) | O4—V5—O10 | 98.12 (9) |
O8—V1—O14 | 80.26 (8) | O11—V5—O10 | 94.90 (9) |
O13ii—V1—O14 | 75.53 (7) | O13—V5—O10 | 155.56 (9) |
O10—V1—O14 | 76.79 (7) | O4—V5—O14ii | 89.35 (9) |
O1—V1—V3ii | 89.53 (8) | O11—V5—O14ii | 164.47 (9) |
O5—V1—V3ii | 128.65 (7) | O13—V5—O14ii | 81.52 (8) |
O8—V1—V3ii | 130.08 (7) | O10—V5—O14ii | 81.38 (8) |
O13ii—V1—V3ii | 40.28 (6) | O4—V5—O14 | 167.59 (9) |
O10—V1—V3ii | 39.42 (6) | O11—V5—O14 | 86.27 (9) |
O14—V1—V3ii | 85.11 (5) | O13—V5—O14 | 79.71 (8) |
O1—V1—V4 | 134.89 (8) | O10—V5—O14 | 79.81 (8) |
O5—V1—V4 | 83.25 (7) | O14ii—V5—O14 | 78.24 (8) |
O8—V1—V4 | 33.44 (6) | O4—V5—V4ii | 40.92 (7) |
O13ii—V1—V4 | 88.32 (6) | O11—V5—V4ii | 147.04 (7) |
O10—V1—V4 | 124.52 (6) | O13—V5—V4ii | 90.78 (6) |
O14—V1—V4 | 47.73 (5) | O10—V5—V4ii | 90.83 (6) |
V3ii—V1—V4 | 121.00 (2) | O14ii—V5—V4ii | 48.43 (5) |
O2—V2—O6 | 103.25 (11) | O14—V5—V4ii | 126.68 (5) |
O2—V2—O9 | 103.41 (11) | O4—V5—V2 | 143.01 (7) |
O6—V2—O9 | 90.59 (9) | O11—V5—V2 | 36.89 (7) |
O2—V2—O5 | 102.27 (11) | O13—V5—V2 | 87.90 (6) |
O6—V2—O5 | 153.96 (9) | O10—V5—V2 | 88.83 (6) |
O9—V2—O5 | 88.49 (9) | O14ii—V5—V2 | 127.64 (6) |
O2—V2—O11 | 101.11 (10) | O14—V5—V2 | 49.40 (5) |
O6—V2—O11 | 86.34 (9) | V4ii—V5—V2 | 176.05 (2) |
O9—V2—O11 | 155.34 (9) | V5—O4—V4ii | 107.67 (10) |
O5—V2—O11 | 83.76 (9) | V1—O5—V2 | 114.96 (10) |
O2—V2—O14 | 176.41 (10) | V3—O6—V2 | 115.83 (11) |
O6—V2—O14 | 77.59 (8) | V1—O8—V4 | 113.96 (11) |
O9—V2—O14 | 80.03 (8) | V4—O9—V2 | 114.16 (11) |
O5—V2—O14 | 76.63 (8) | V5—O10—V3ii | 106.27 (9) |
O11—V2—O14 | 75.41 (7) | V5—O10—V1 | 107.93 (9) |
O2—V2—V5 | 131.81 (9) | V3ii—O10—V1 | 100.69 (9) |
O6—V2—V5 | 79.82 (6) | V5—O11—V2 | 112.40 (11) |
O9—V2—V5 | 124.76 (7) | V3—O12—V4 | 113.98 (10) |
O5—V2—V5 | 79.40 (6) | V5—O13—V1ii | 106.31 (9) |
O11—V2—V5 | 30.71 (6) | V5—O13—V3 | 109.36 (9) |
O14—V2—V5 | 44.73 (5) | V1ii—O13—V3 | 99.84 (9) |
O2—V2—V4 | 135.82 (9) | V5ii—O14—V5 | 101.76 (8) |
O6—V2—V4 | 83.31 (7) | V5ii—O14—V1 | 93.52 (8) |
O9—V2—V4 | 32.41 (6) | V5—O14—V1 | 93.07 (7) |
O5—V2—V4 | 82.05 (6) | V5ii—O14—V3 | 93.37 (7) |
O11—V2—V4 | 123.01 (6) | V5—O14—V3 | 93.16 (7) |
O14—V2—V4 | 47.63 (5) | V1—O14—V3 | 169.59 (9) |
V5—V2—V4 | 92.353 (18) | V5ii—O14—V4 | 89.03 (7) |
O7—V3—O12 | 103.53 (10) | V5—O14—V4 | 169.21 (9) |
O7—V3—O6 | 103.55 (10) | V1—O14—V4 | 86.02 (7) |
O12—V3—O6 | 95.37 (9) | V3—O14—V4 | 86.30 (7) |
O7—V3—O10ii | 99.59 (10) | V5ii—O14—V2 | 172.36 (10) |
O12—V3—O10ii | 90.71 (9) | V5—O14—V2 | 85.87 (7) |
O6—V3—O10ii | 153.92 (9) | V1—O14—V2 | 86.49 (6) |
O7—V3—O13 | 100.05 (10) | V3—O14—V2 | 85.65 (7) |
O12—V3—O13 | 154.65 (9) | V4—O14—V2 | 83.34 (6) |
O6—V3—O13 | 87.99 (9) | H11W—O1W—H12W | 112 (3) |
O10ii—V3—O13 | 76.20 (8) | H21W—O2W—H22W | 108 (3) |
O7—V3—O14 | 174.19 (9) | H31W—O3W—H32W | 110 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N11—H1A···O8iii | 0.89 | 1.89 | 2.785 (3) | 178 |
N11—H1B···O1Wiv | 0.89 | 2.05 | 2.817 (4) | 144 |
N11—H1C···O1Wi | 0.89 | 1.97 | 2.845 (4) | 167 |
N12—H2A···O3Wv | 0.89 | 1.84 | 2.729 (4) | 173 |
N12—H2B···O10 | 0.89 | 1.93 | 2.810 (3) | 168 |
N12—H2C···O3iii | 0.89 | 2.58 | 3.308 (4) | 140 |
N12—H2C···O5 | 0.89 | 2.54 | 2.938 (4) | 108 |
N2—H21N···O12iii | 0.89 | 1.92 | 2.815 (3) | 179 |
N2—H22N···O1vi | 0.89 | 2.34 | 2.890 (3) | 120 |
N2—H22N···O7vii | 0.89 | 2.24 | 3.076 (3) | 156 |
N2—H23N···O2 | 0.89 | 2.15 | 3.019 (4) | 164 |
O1W—H11W···O13vii | 0.83 (2) | 1.89 (2) | 2.716 (3) | 175 (4) |
O1W—H12W···O2W | 0.83 (2) | 1.95 (2) | 2.748 (3) | 161 (3) |
O2W—H21W···O6vii | 0.84 (2) | 2.01 (2) | 2.774 (3) | 152 (4) |
O2W—H22W···O5i | 0.85 (2) | 1.95 (2) | 2.780 (3) | 165 (4) |
O3W—H31W···O9i | 0.84 (2) | 1.94 (2) | 2.744 (3) | 162 (4) |
O3W—H32W···O2W | 0.83 (2) | 2.05 (2) | 2.833 (4) | 157 (4) |
C13—H13B···O3iii | 0.97 | 2.50 | 3.409 (4) | 155 |
C13—H13B···O8iii | 0.97 | 2.58 | 3.217 (4) | 123 |
C14—H14B···O1 | 0.97 | 2.49 | 3.270 (4) | 137 |
C21—H21A···O3W | 0.97 | 2.56 | 3.335 (4) | 136 |
C21—H21B···O3iii | 0.97 | 2.57 | 3.216 (4) | 124 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (iii) x−1/2, −y+1/2, z+1/2; (iv) x−1, y, z; (v) −x+1/2, y−1/2, −z+3/2; (vi) x+1/2, −y+1/2, z+1/2; (vii) −x+3/2, y+1/2, −z+3/2. |
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