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In the title compound, [Mn(C12H8N2)2(H2O)2][NbOF5], each of the MnII and NbV atoms has a distorted octahedral coordination. In the [NbOF5]2− anion, a characteristic short terminal Nb=O bond and a longer Nb—F bond are observed, which result in the out-of-center distortion of the octahedron, a manifestation of the second-order Jahn–Teller effect.
Supporting information
CCDC reference: 290543
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.006 Å
- R factor = 0.033
- wR factor = 0.092
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Nb1
PLAT432_ALERT_2_C Short Inter X...Y Contact F4 .. C22 .. 2.93 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact O3 .. C10 .. 2.97 Ang.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 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
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SMART; data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXTL.
Diaquabis(1,10-phenanthroline-
κ2N,
N')manganese(II)
pentafluorooxoniobate
top
Crystal data top
[Mn(C12H8N2)2(H2O)2][NbF5O] | Z = 2 |
Mr = 655.29 | F(000) = 654 |
Triclinic, P1 | Dx = 1.702 Mg m−3 |
a = 9.6242 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.3971 (5) Å | Cell parameters from 2712 reflections |
c = 13.0605 (5) Å | θ = 1.7–25.1° |
α = 72.341 (2)° | µ = 1.01 mm−1 |
β = 70.054 (3)° | T = 273 K |
γ = 79.686 (3)° | Block, yellow |
V = 1278.62 (9) Å3 | 0.31 × 0.20 × 0.07 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 4530 independent reflections |
Radiation source: fine-focus sealed tube | 3265 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 25.1°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −11→11 |
Tmin = 0.746, Tmax = 0.937 | k = −13→13 |
12791 measured reflections | l = −15→15 |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0507P)2] where P = (Fo2 + 2Fc2)/3 |
4530 reflections | (Δ/σ)max = 0.001 |
360 parameters | Δρmax = 0.46 e Å−3 |
4 restraints | Δρmin = −0.53 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 | |
Nb1 | 0.88497 (4) | 0.23500 (3) | 0.18405 (3) | 0.04906 (14) | |
Mn1 | 0.20835 (6) | 0.27630 (4) | 0.77626 (4) | 0.04110 (15) | |
F1 | 0.9318 (4) | 0.1226 (2) | 0.3103 (2) | 0.1177 (12) | |
F2 | 0.6788 (3) | 0.2382 (3) | 0.2574 (3) | 0.1104 (10) | |
F3 | 0.8380 (3) | 0.32686 (18) | 0.04452 (18) | 0.0724 (6) | |
F4 | 1.0861 (3) | 0.2096 (3) | 0.0912 (3) | 0.1061 (9) | |
F5 | 0.8680 (3) | 0.08464 (19) | 0.1351 (2) | 0.0955 (9) | |
N1 | 0.1467 (3) | 0.2509 (2) | 0.6331 (2) | 0.0498 (7) | |
N2 | 0.2837 (3) | 0.4425 (2) | 0.6269 (2) | 0.0491 (7) | |
N3 | 0.4117 (3) | 0.1365 (2) | 0.7558 (2) | 0.0467 (7) | |
N4 | 0.3401 (3) | 0.3066 (2) | 0.8772 (2) | 0.0461 (7) | |
O1 | 0.0231 (3) | 0.4002 (2) | 0.8372 (2) | 0.0497 (6) | |
O2 | 0.0813 (3) | 0.1308 (2) | 0.8975 (2) | 0.0557 (6) | |
O3 | 0.9179 (3) | 0.36735 (19) | 0.2116 (2) | 0.0621 (7) | |
C1 | 0.0795 (5) | 0.1572 (3) | 0.6357 (4) | 0.0690 (11) | |
H1A | 0.0609 | 0.0919 | 0.7005 | 0.083* | |
C2 | 0.0358 (5) | 0.1522 (4) | 0.5462 (4) | 0.0800 (13) | |
H2A | −0.0099 | 0.0845 | 0.5510 | 0.096* | |
C3 | 0.0606 (5) | 0.2471 (5) | 0.4522 (4) | 0.0833 (14) | |
H3 | 0.0314 | 0.2449 | 0.3919 | 0.100* | |
C4 | 0.1295 (5) | 0.3482 (4) | 0.4445 (3) | 0.0674 (11) | |
C5 | 0.1571 (6) | 0.4538 (5) | 0.3491 (4) | 0.0895 (15) | |
H5 | 0.1322 | 0.4553 | 0.2859 | 0.107* | |
C6 | 0.2180 (6) | 0.5505 (5) | 0.3492 (4) | 0.0922 (16) | |
H6 | 0.2317 | 0.6188 | 0.2869 | 0.111* | |
C7 | 0.2619 (4) | 0.5512 (4) | 0.4417 (3) | 0.0666 (11) | |
C8 | 0.3248 (5) | 0.6505 (4) | 0.4469 (4) | 0.0861 (15) | |
H8 | 0.3371 | 0.7218 | 0.3875 | 0.103* | |
C9 | 0.3677 (5) | 0.6439 (4) | 0.5366 (4) | 0.0783 (14) | |
H9 | 0.4115 | 0.7092 | 0.5386 | 0.094* | |
C10 | 0.3454 (4) | 0.5374 (3) | 0.6266 (3) | 0.0600 (10) | |
H10 | 0.3751 | 0.5332 | 0.6885 | 0.072* | |
C11 | 0.2418 (4) | 0.4486 (3) | 0.5360 (3) | 0.0497 (9) | |
C12 | 0.1724 (4) | 0.3459 (3) | 0.5382 (3) | 0.0500 (9) | |
C13 | 0.4458 (5) | 0.0517 (3) | 0.6990 (3) | 0.0667 (11) | |
H13 | 0.3858 | 0.0506 | 0.6566 | 0.080* | |
C14 | 0.5660 (5) | −0.0354 (4) | 0.6992 (4) | 0.0814 (13) | |
H14 | 0.5857 | −0.0930 | 0.6576 | 0.098* | |
C15 | 0.6556 (5) | −0.0360 (4) | 0.7613 (4) | 0.0771 (12) | |
H15 | 0.7375 | −0.0933 | 0.7613 | 0.092* | |
C16 | 0.6230 (4) | 0.0500 (3) | 0.8245 (3) | 0.0579 (10) | |
C17 | 0.7071 (5) | 0.0532 (4) | 0.8949 (4) | 0.0761 (12) | |
H17 | 0.7892 | −0.0033 | 0.8981 | 0.091* | |
C18 | 0.6710 (5) | 0.1353 (4) | 0.9564 (4) | 0.0740 (12) | |
H18 | 0.7285 | 0.1358 | 1.0007 | 0.089* | |
C19 | 0.5445 (4) | 0.2222 (3) | 0.9542 (3) | 0.0548 (9) | |
C20 | 0.4998 (5) | 0.3084 (4) | 1.0192 (4) | 0.0691 (11) | |
H20 | 0.5520 | 0.3097 | 1.0671 | 0.083* | |
C21 | 0.3797 (5) | 0.3900 (4) | 1.0114 (4) | 0.0684 (11) | |
H21 | 0.3491 | 0.4476 | 1.0537 | 0.082* | |
C22 | 0.3030 (4) | 0.3865 (3) | 0.9398 (3) | 0.0585 (10) | |
H22 | 0.2213 | 0.4432 | 0.9354 | 0.070* | |
C23 | 0.4600 (4) | 0.2241 (3) | 0.8851 (3) | 0.0449 (8) | |
C24 | 0.4994 (4) | 0.1347 (3) | 0.8194 (3) | 0.0450 (8) | |
H2C | 0.091 (4) | 0.0578 (19) | 0.892 (3) | 0.055 (10)* | |
H2D | 0.039 (5) | 0.131 (5) | 0.964 (2) | 0.12 (2)* | |
H1C | −0.036 (4) | 0.380 (3) | 0.904 (2) | 0.066 (13)* | |
H1D | 0.036 (5) | 0.474 (2) | 0.822 (4) | 0.102 (17)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nb1 | 0.0656 (3) | 0.03648 (17) | 0.0506 (2) | 0.00268 (14) | −0.02357 (17) | −0.01656 (13) |
Mn1 | 0.0532 (3) | 0.0317 (2) | 0.0459 (3) | −0.0003 (2) | −0.0256 (3) | −0.0109 (2) |
F1 | 0.243 (4) | 0.0507 (13) | 0.0962 (19) | −0.0231 (18) | −0.109 (2) | 0.0000 (13) |
F2 | 0.0776 (19) | 0.144 (2) | 0.117 (2) | −0.0470 (17) | 0.0095 (16) | −0.067 (2) |
F3 | 0.0922 (18) | 0.0596 (12) | 0.0628 (14) | 0.0076 (12) | −0.0342 (13) | −0.0084 (10) |
F4 | 0.0708 (18) | 0.109 (2) | 0.129 (2) | 0.0265 (15) | −0.0189 (16) | −0.0502 (18) |
F5 | 0.168 (3) | 0.0451 (11) | 0.113 (2) | 0.0069 (14) | −0.089 (2) | −0.0342 (12) |
N1 | 0.066 (2) | 0.0424 (15) | 0.0525 (18) | 0.0012 (14) | −0.0314 (15) | −0.0170 (13) |
N2 | 0.0573 (19) | 0.0364 (14) | 0.0507 (18) | 0.0035 (13) | −0.0146 (15) | −0.0138 (12) |
N3 | 0.0508 (18) | 0.0378 (14) | 0.0562 (18) | 0.0020 (12) | −0.0208 (15) | −0.0172 (13) |
N4 | 0.0523 (18) | 0.0375 (14) | 0.0556 (18) | −0.0011 (13) | −0.0257 (14) | −0.0134 (12) |
O1 | 0.0583 (17) | 0.0351 (13) | 0.0536 (17) | 0.0034 (12) | −0.0200 (14) | −0.0095 (11) |
O2 | 0.0773 (19) | 0.0344 (13) | 0.0560 (18) | −0.0093 (12) | −0.0154 (14) | −0.0159 (12) |
O3 | 0.0744 (18) | 0.0383 (12) | 0.0869 (19) | −0.0045 (12) | −0.0325 (15) | −0.0263 (12) |
C1 | 0.098 (3) | 0.051 (2) | 0.079 (3) | −0.004 (2) | −0.048 (3) | −0.0254 (19) |
C2 | 0.102 (4) | 0.077 (3) | 0.098 (4) | 0.004 (3) | −0.064 (3) | −0.044 (3) |
C3 | 0.083 (3) | 0.117 (4) | 0.081 (3) | 0.023 (3) | −0.055 (3) | −0.055 (3) |
C4 | 0.065 (3) | 0.091 (3) | 0.051 (2) | 0.018 (2) | −0.031 (2) | −0.025 (2) |
C5 | 0.084 (4) | 0.130 (4) | 0.045 (3) | 0.015 (3) | −0.035 (2) | −0.008 (3) |
C6 | 0.084 (4) | 0.105 (4) | 0.050 (3) | 0.013 (3) | −0.016 (3) | 0.014 (3) |
C7 | 0.053 (3) | 0.069 (3) | 0.051 (2) | 0.008 (2) | −0.0052 (19) | 0.0015 (19) |
C8 | 0.076 (3) | 0.063 (3) | 0.076 (3) | 0.000 (2) | 0.006 (3) | 0.008 (2) |
C9 | 0.071 (3) | 0.048 (2) | 0.088 (3) | −0.012 (2) | 0.011 (3) | −0.014 (2) |
C10 | 0.058 (2) | 0.0466 (19) | 0.066 (3) | −0.0060 (17) | −0.0009 (19) | −0.0216 (18) |
C11 | 0.042 (2) | 0.0495 (19) | 0.045 (2) | 0.0111 (16) | −0.0080 (16) | −0.0094 (15) |
C12 | 0.050 (2) | 0.056 (2) | 0.044 (2) | 0.0163 (17) | −0.0213 (17) | −0.0168 (16) |
C13 | 0.069 (3) | 0.063 (2) | 0.077 (3) | 0.003 (2) | −0.026 (2) | −0.032 (2) |
C14 | 0.080 (3) | 0.062 (2) | 0.104 (4) | 0.017 (2) | −0.022 (3) | −0.045 (2) |
C15 | 0.056 (3) | 0.066 (3) | 0.107 (4) | 0.017 (2) | −0.028 (3) | −0.029 (2) |
C16 | 0.051 (2) | 0.0470 (19) | 0.072 (3) | 0.0052 (17) | −0.023 (2) | −0.0117 (18) |
C17 | 0.060 (3) | 0.070 (3) | 0.097 (4) | 0.017 (2) | −0.041 (3) | −0.014 (2) |
C18 | 0.062 (3) | 0.076 (3) | 0.095 (3) | 0.007 (2) | −0.049 (3) | −0.017 (2) |
C19 | 0.053 (2) | 0.0534 (19) | 0.063 (2) | −0.0038 (17) | −0.031 (2) | −0.0066 (17) |
C20 | 0.081 (3) | 0.070 (3) | 0.079 (3) | −0.012 (2) | −0.052 (2) | −0.018 (2) |
C21 | 0.084 (3) | 0.063 (2) | 0.084 (3) | −0.005 (2) | −0.043 (3) | −0.036 (2) |
C22 | 0.065 (3) | 0.0469 (19) | 0.079 (3) | 0.0014 (17) | −0.042 (2) | −0.0203 (18) |
C23 | 0.048 (2) | 0.0355 (16) | 0.051 (2) | −0.0082 (15) | −0.0218 (17) | −0.0019 (14) |
C24 | 0.042 (2) | 0.0366 (16) | 0.051 (2) | −0.0052 (15) | −0.0157 (16) | −0.0007 (14) |
Geometric parameters (Å, º) top
Nb1—O3 | 1.756 (2) | C5—C6 | 1.337 (6) |
Nb1—F2 | 1.885 (3) | C5—H5 | 0.9300 |
Nb1—F1 | 1.892 (2) | C6—C7 | 1.413 (7) |
Nb1—F4 | 1.927 (3) | C6—H6 | 0.9300 |
Nb1—F3 | 1.964 (2) | C7—C11 | 1.401 (5) |
Nb1—F5 | 2.0516 (19) | C7—C8 | 1.404 (6) |
Mn1—O2 | 2.137 (3) | C8—C9 | 1.347 (6) |
Mn1—O1 | 2.149 (2) | C8—H8 | 0.9300 |
Mn1—N4 | 2.245 (3) | C9—C10 | 1.399 (5) |
Mn1—N1 | 2.254 (3) | C9—H9 | 0.9300 |
Mn1—N2 | 2.281 (3) | C10—H10 | 0.9300 |
Mn1—N3 | 2.286 (3) | C11—C12 | 1.437 (5) |
N1—C1 | 1.330 (4) | C13—C14 | 1.384 (6) |
N1—C12 | 1.357 (4) | C13—H13 | 0.9300 |
N2—C10 | 1.322 (4) | C14—C15 | 1.367 (6) |
N2—C11 | 1.358 (4) | C14—H14 | 0.9300 |
N3—C13 | 1.321 (4) | C15—C16 | 1.395 (6) |
N3—C24 | 1.366 (4) | C15—H15 | 0.9300 |
N4—C22 | 1.327 (4) | C16—C24 | 1.398 (5) |
N4—C23 | 1.364 (4) | C16—C17 | 1.429 (6) |
O1—H1C | 0.849 (18) | C17—C18 | 1.338 (6) |
O1—H1D | 0.826 (19) | C17—H17 | 0.9300 |
O2—H2C | 0.841 (18) | C18—C19 | 1.428 (5) |
O2—H2D | 0.825 (19) | C18—H18 | 0.9300 |
C1—C2 | 1.390 (5) | C19—C23 | 1.399 (5) |
C1—H1A | 0.9300 | C19—C20 | 1.407 (5) |
C2—C3 | 1.350 (6) | C20—C21 | 1.360 (6) |
C2—H2A | 0.9300 | C20—H20 | 0.9300 |
C3—C4 | 1.391 (6) | C21—C22 | 1.387 (5) |
C3—H3 | 0.9300 | C21—H21 | 0.9300 |
C4—C12 | 1.410 (5) | C22—H22 | 0.9300 |
C4—C5 | 1.432 (6) | C23—C24 | 1.445 (5) |
| | | |
O3—Nb1—F2 | 98.01 (12) | C6—C5—C4 | 121.3 (4) |
O3—Nb1—F1 | 95.18 (11) | C6—C5—H5 | 119.4 |
F2—Nb1—F1 | 93.64 (16) | C4—C5—H5 | 119.4 |
O3—Nb1—F4 | 93.98 (12) | C5—C6—C7 | 121.5 (4) |
F2—Nb1—F4 | 167.12 (12) | C5—C6—H6 | 119.2 |
F1—Nb1—F4 | 89.93 (14) | C7—C6—H6 | 119.2 |
O3—Nb1—F3 | 94.22 (11) | C11—C7—C8 | 116.4 (4) |
F2—Nb1—F3 | 87.14 (13) | C11—C7—C6 | 119.7 (4) |
F1—Nb1—F3 | 170.37 (9) | C8—C7—C6 | 123.9 (4) |
F4—Nb1—F3 | 87.32 (12) | C9—C8—C7 | 120.9 (4) |
O3—Nb1—F5 | 173.18 (12) | C9—C8—H8 | 119.6 |
F2—Nb1—F5 | 88.04 (12) | C7—C8—H8 | 119.6 |
F1—Nb1—F5 | 87.53 (9) | C8—C9—C10 | 119.1 (4) |
F4—Nb1—F5 | 79.74 (12) | C8—C9—H9 | 120.5 |
F3—Nb1—F5 | 82.91 (9) | C10—C9—H9 | 120.5 |
O2—Mn1—O1 | 86.23 (10) | N2—C10—C9 | 122.3 (4) |
O2—Mn1—N4 | 100.20 (10) | N2—C10—H10 | 118.8 |
O1—Mn1—N4 | 93.83 (10) | C9—C10—H10 | 118.8 |
O2—Mn1—N1 | 93.04 (10) | N2—C11—C7 | 122.7 (4) |
O1—Mn1—N1 | 99.39 (10) | N2—C11—C12 | 118.1 (3) |
N4—Mn1—N1 | 161.86 (11) | C7—C11—C12 | 119.2 (4) |
O2—Mn1—N2 | 162.58 (11) | N1—C12—C4 | 122.3 (3) |
O1—Mn1—N2 | 85.17 (10) | N1—C12—C11 | 118.0 (3) |
N4—Mn1—N2 | 95.46 (10) | C4—C12—C11 | 119.7 (3) |
N1—Mn1—N2 | 73.51 (10) | N3—C13—C14 | 123.4 (4) |
O2—Mn1—N3 | 88.46 (10) | N3—C13—H13 | 118.3 |
O1—Mn1—N3 | 165.41 (10) | C14—C13—H13 | 118.3 |
N4—Mn1—N3 | 73.74 (10) | C15—C14—C13 | 119.4 (4) |
N1—Mn1—N3 | 94.45 (10) | C15—C14—H14 | 120.3 |
N2—Mn1—N3 | 103.30 (10) | C13—C14—H14 | 120.3 |
C1—N1—C12 | 117.8 (3) | C14—C15—C16 | 119.5 (4) |
C1—N1—Mn1 | 126.5 (2) | C14—C15—H15 | 120.3 |
C12—N1—Mn1 | 115.5 (2) | C16—C15—H15 | 120.3 |
C10—N2—C11 | 118.6 (3) | C15—C16—C24 | 117.3 (4) |
C10—N2—Mn1 | 126.4 (3) | C15—C16—C17 | 123.3 (4) |
C11—N2—Mn1 | 114.4 (2) | C24—C16—C17 | 119.4 (4) |
C13—N3—C24 | 117.3 (3) | C18—C17—C16 | 121.8 (4) |
C13—N3—Mn1 | 128.0 (3) | C18—C17—H17 | 119.1 |
C24—N3—Mn1 | 114.5 (2) | C16—C17—H17 | 119.1 |
C22—N4—C23 | 117.4 (3) | C17—C18—C19 | 120.3 (4) |
C22—N4—Mn1 | 126.4 (2) | C17—C18—H18 | 119.8 |
C23—N4—Mn1 | 115.7 (2) | C19—C18—H18 | 119.8 |
Mn1—O1—H1C | 121 (3) | C23—C19—C20 | 117.5 (3) |
Mn1—O1—H1D | 118 (3) | C23—C19—C18 | 120.0 (4) |
H1C—O1—H1D | 108 (4) | C20—C19—C18 | 122.5 (4) |
Mn1—O2—H2C | 125 (2) | C21—C20—C19 | 119.3 (4) |
Mn1—O2—H2D | 124 (4) | C21—C20—H20 | 120.3 |
H2C—O2—H2D | 109 (4) | C19—C20—H20 | 120.3 |
N1—C1—C2 | 123.2 (4) | C20—C21—C22 | 119.6 (4) |
N1—C1—H1A | 118.4 | C20—C21—H21 | 120.2 |
C2—C1—H1A | 118.4 | C22—C21—H21 | 120.2 |
C3—C2—C1 | 118.9 (4) | N4—C22—C21 | 123.4 (4) |
C3—C2—H2A | 120.5 | N4—C22—H22 | 118.3 |
C1—C2—H2A | 120.5 | C21—C22—H22 | 118.3 |
C2—C3—C4 | 120.7 (4) | N4—C23—C19 | 122.8 (3) |
C2—C3—H3 | 119.7 | N4—C23—C24 | 117.9 (3) |
C4—C3—H3 | 119.7 | C19—C23—C24 | 119.3 (3) |
C3—C4—C12 | 117.1 (4) | N3—C24—C16 | 123.0 (3) |
C3—C4—C5 | 124.3 (4) | N3—C24—C23 | 117.7 (3) |
C12—C4—C5 | 118.6 (4) | C16—C24—C23 | 119.2 (3) |
| | | |
O2—Mn1—N1—C1 | −11.3 (3) | C10—N2—C11—C7 | 0.3 (5) |
O1—Mn1—N1—C1 | −97.9 (3) | Mn1—N2—C11—C7 | 172.1 (3) |
N4—Mn1—N1—C1 | 125.8 (4) | C10—N2—C11—C12 | −178.9 (3) |
N2—Mn1—N1—C1 | 180.0 (3) | Mn1—N2—C11—C12 | −7.1 (4) |
N3—Mn1—N1—C1 | 77.4 (3) | C8—C7—C11—N2 | −1.7 (5) |
O2—Mn1—N1—C12 | 163.9 (2) | C6—C7—C11—N2 | 178.9 (4) |
O1—Mn1—N1—C12 | 77.2 (2) | C8—C7—C11—C12 | 177.5 (3) |
N4—Mn1—N1—C12 | −59.0 (4) | C6—C7—C11—C12 | −1.9 (5) |
N2—Mn1—N1—C12 | −4.8 (2) | C1—N1—C12—C4 | 0.6 (5) |
N3—Mn1—N1—C12 | −107.4 (2) | Mn1—N1—C12—C4 | −175.0 (3) |
O2—Mn1—N2—C10 | 136.7 (4) | C1—N1—C12—C11 | 178.6 (3) |
O1—Mn1—N2—C10 | 76.0 (3) | Mn1—N1—C12—C11 | 2.9 (4) |
N4—Mn1—N2—C10 | −17.4 (3) | C3—C4—C12—N1 | −1.0 (6) |
N1—Mn1—N2—C10 | 177.3 (3) | C5—C4—C12—N1 | 178.2 (4) |
N3—Mn1—N2—C10 | −91.9 (3) | C3—C4—C12—C11 | −178.9 (3) |
O2—Mn1—N2—C11 | −34.4 (5) | C5—C4—C12—C11 | 0.2 (5) |
O1—Mn1—N2—C11 | −95.0 (2) | N2—C11—C12—N1 | 2.9 (5) |
N4—Mn1—N2—C11 | 171.6 (2) | C7—C11—C12—N1 | −176.3 (3) |
N1—Mn1—N2—C11 | 6.3 (2) | N2—C11—C12—C4 | −179.0 (3) |
N3—Mn1—N2—C11 | 97.0 (2) | C7—C11—C12—C4 | 1.8 (5) |
O2—Mn1—N3—C13 | 77.3 (3) | C24—N3—C13—C14 | −1.4 (6) |
O1—Mn1—N3—C13 | 145.9 (4) | Mn1—N3—C13—C14 | −174.6 (3) |
N4—Mn1—N3—C13 | 178.4 (3) | N3—C13—C14—C15 | 0.3 (7) |
N1—Mn1—N3—C13 | −15.6 (3) | C13—C14—C15—C16 | 0.9 (7) |
N2—Mn1—N3—C13 | −89.7 (3) | C14—C15—C16—C24 | −0.9 (6) |
O2—Mn1—N3—C24 | −96.0 (2) | C14—C15—C16—C17 | 177.6 (4) |
O1—Mn1—N3—C24 | −27.4 (5) | C15—C16—C17—C18 | −178.5 (4) |
N4—Mn1—N3—C24 | 5.1 (2) | C24—C16—C17—C18 | −0.1 (6) |
N1—Mn1—N3—C24 | 171.0 (2) | C16—C17—C18—C19 | 0.8 (7) |
N2—Mn1—N3—C24 | 96.9 (2) | C17—C18—C19—C23 | −1.8 (6) |
O2—Mn1—N4—C22 | −92.1 (3) | C17—C18—C19—C20 | 178.5 (4) |
O1—Mn1—N4—C22 | −5.2 (3) | C23—C19—C20—C21 | −0.9 (6) |
N1—Mn1—N4—C22 | 131.6 (3) | C18—C19—C20—C21 | 178.8 (4) |
N2—Mn1—N4—C22 | 80.3 (3) | C19—C20—C21—C22 | 0.2 (6) |
N3—Mn1—N4—C22 | −177.5 (3) | C23—N4—C22—C21 | 0.2 (5) |
O2—Mn1—N4—C23 | 79.4 (2) | Mn1—N4—C22—C21 | 171.5 (3) |
O1—Mn1—N4—C23 | 166.2 (2) | C20—C21—C22—N4 | 0.2 (6) |
N1—Mn1—N4—C23 | −56.9 (4) | C22—N4—C23—C19 | −1.0 (5) |
N2—Mn1—N4—C23 | −108.3 (2) | Mn1—N4—C23—C19 | −173.3 (3) |
N3—Mn1—N4—C23 | −6.0 (2) | C22—N4—C23—C24 | 178.6 (3) |
C12—N1—C1—C2 | 0.3 (6) | Mn1—N4—C23—C24 | 6.3 (4) |
Mn1—N1—C1—C2 | 175.4 (3) | C20—C19—C23—N4 | 1.3 (5) |
N1—C1—C2—C3 | −0.8 (7) | C18—C19—C23—N4 | −178.4 (3) |
C1—C2—C3—C4 | 0.3 (7) | C20—C19—C23—C24 | −178.2 (3) |
C2—C3—C4—C12 | 0.5 (6) | C18—C19—C23—C24 | 2.0 (5) |
C2—C3—C4—C5 | −178.6 (4) | C13—N3—C24—C16 | 1.4 (5) |
C3—C4—C5—C6 | 177.0 (5) | Mn1—N3—C24—C16 | 175.5 (3) |
C12—C4—C5—C6 | −2.1 (7) | C13—N3—C24—C23 | −177.8 (3) |
C4—C5—C6—C7 | 1.9 (8) | Mn1—N3—C24—C23 | −3.7 (4) |
C5—C6—C7—C11 | 0.1 (7) | C15—C16—C24—N3 | −0.3 (5) |
C5—C6—C7—C8 | −179.3 (5) | C17—C16—C24—N3 | −178.8 (3) |
C11—C7—C8—C9 | 2.3 (6) | C15—C16—C24—C23 | 178.9 (3) |
C6—C7—C8—C9 | −178.3 (4) | C17—C16—C24—C23 | 0.4 (5) |
C7—C8—C9—C10 | −1.6 (7) | N4—C23—C24—N3 | −1.7 (4) |
C11—N2—C10—C9 | 0.6 (5) | C19—C23—C24—N3 | 177.9 (3) |
Mn1—N2—C10—C9 | −170.1 (3) | N4—C23—C24—C16 | 179.1 (3) |
C8—C9—C10—N2 | 0.1 (6) | C19—C23—C24—C16 | −1.4 (5) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1C···F3i | 0.85 (3) | 1.81 (3) | 2.660 (3) | 176 (4) |
O1—H1D···O3ii | 0.83 (3) | 1.83 (3) | 2.649 (3) | 175 (5) |
O2—H2C···F5iii | 0.84 (2) | 1.72 (2) | 2.552 (3) | 172 (3) |
O2—H2D···F4i | 0.82 (3) | 2.31 (4) | 2.947 (4) | 135 (4) |
O2—H2D···F5i | 0.82 (3) | 2.25 (3) | 3.028 (3) | 157 (5) |
C1—H1A···F1iii | 0.93 | 2.48 | 3.064 (4) | 121 |
C3—H3···F1iv | 0.93 | 2.46 | 3.283 (6) | 147 |
C5—H5···O1v | 0.93 | 2.59 | 3.330 (6) | 137 |
C17—H17···F4vi | 0.93 | 2.43 | 3.278 (6) | 152 |
C18—H18···F5vii | 0.93 | 2.44 | 3.344 (6) | 166 |
Symmetry codes: (i) x−1, y, z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) x−1, y, z; (v) −x, −y+1, −z+1; (vi) −x+2, −y, −z+1; (vii) x, y, z+1. |
Bond valence paremeters top | Si | V—Si |
Nb1—O3 | 1.52 | 0.48 |
Nb1—F2 | 0.84 | 0.16 |
Nb1—F1 | 0.83 | 0.17 |
Nb1—F4 | 0.75 | 0.25 |
Nb1—F3 | 0.68 | 0.32 |
Nb1—F5 | 0.54 | 0.46 |
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