The crystal structure of the title compound, [Mn(TPP)(η
1-H
2Btz
2)(H
2O)]·H
2O [where H
2Btz = dihydrobis(1,2,4-triazolyl)borate, C
4H
6BN
6, and TPP = tetraphenylporphyrin, C
44H
20N
4], contains a singly coordinated H
2Btz
2. The TPP ligand is highly distorted even though the coordination environment around Mn
III has regular octahedral geometry. Both coordinated and uncoordinated water molecules are involved in intermolecular hydrogen bond through O—H
O, O—H
N and O—H
(π-arene) interactions to form a three-dimensional network.
Supporting information
CCDC reference: 245106
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.004 Å
- R factor = 0.044
- wR factor = 0.105
- Data-to-parameter ratio = 12.8
checkCIF/PLATON results
No syntax errors found
Datablock: I
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O1W - H1W ... ?
Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for N5 - C46 .. 5.20 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for N10 - C48 .. 5.43 su
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1W .. CG1 .. 2.90 Ang.
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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
Data collection: COLLECT (Nonius, 1997-2002); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Crystal data top
[Mn(C44H20N4)(C4H6BN6)(H2O)](H2O) | F(000) = 1768 |
Mr = 852.63 | Dx = 1.345 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 37308 reflections |
a = 12.2498 (2) Å | θ = 2.7–25.0° |
b = 16.0805 (5) Å | µ = 0.37 mm−1 |
c = 21.5391 (6) Å | T = 100 K |
β = 96.944 (2)° | Plate, dark green |
V = 4211.71 (19) Å3 | 0.30 × 0.30 × 0.15 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD area-detector diffractometer | 7423 independent reflections |
Radiation source: fine-focus sealed tube | 5034 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.063 |
Detector resolution: 9 pixels mm-1 | θmax = 25.0°, θmin = 2.7° |
φ scans and ω scans with κ offsets | h = −14→14 |
Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997) | k = −19→19 |
Tmin = 0.898, Tmax = 0.947 | l = −25→25 |
37308 measured reflections | |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0506P)2 + 0.2174P] where P = (Fo2 + 2Fc2)/3 |
7423 reflections | (Δ/σ)max = 0.001 |
581 parameters | Δρmax = 0.34 e Å−3 |
4 restraints | Δρmin = −0.25 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 | |
Mn1 | 0.29121 (3) | 0.19167 (2) | 0.303349 (15) | 0.02305 (12) | |
O1 | 0.14177 (14) | 0.13133 (13) | 0.25468 (8) | 0.0316 (4) | |
H1O | 0.152 (3) | 0.0803 (5) | 0.2492 (15) | 0.084 (13)* | |
H2O | 0.0778 (8) | 0.1413 (16) | 0.2632 (11) | 0.039 (8)* | |
O1W | −0.07507 (18) | 0.16711 (15) | 0.27508 (11) | 0.0613 (6) | |
H1W | −0.094 (3) | 0.141 (2) | 0.3059 (11) | 0.092* | |
H2W | −0.096 (3) | 0.2169 (7) | 0.2743 (18) | 0.092* | |
N1 | 0.20016 (14) | 0.29351 (12) | 0.31266 (8) | 0.0250 (5) | |
N2 | 0.32888 (14) | 0.23317 (12) | 0.22078 (8) | 0.0230 (5) | |
N3 | 0.37941 (14) | 0.08854 (12) | 0.29361 (8) | 0.0233 (5) | |
N4 | 0.25634 (14) | 0.14991 (13) | 0.38623 (8) | 0.0237 (5) | |
N5 | 0.44176 (15) | 0.26249 (13) | 0.34863 (9) | 0.0261 (5) | |
N6 | 0.54874 (16) | 0.36849 (14) | 0.38805 (9) | 0.0334 (5) | |
N7 | 0.61326 (15) | 0.30494 (13) | 0.37119 (9) | 0.0292 (5) | |
N8 | 0.78611 (15) | 0.36155 (14) | 0.33337 (10) | 0.0315 (5) | |
N9 | 0.81464 (18) | 0.32952 (16) | 0.27855 (11) | 0.0481 (6) | |
N10 | 0.83318 (17) | 0.46968 (17) | 0.27929 (13) | 0.0508 (7) | |
C1 | 0.10042 (19) | 0.39656 (17) | 0.35323 (11) | 0.0341 (7) | |
H1A | 0.0640 | 0.4278 | 0.3820 | 0.041* | |
C2 | 0.10891 (18) | 0.41762 (17) | 0.29341 (12) | 0.0342 (7) | |
H2A | 0.0783 | 0.4655 | 0.2721 | 0.041* | |
C3 | 0.17286 (18) | 0.35428 (16) | 0.26789 (11) | 0.0274 (6) | |
C4 | 0.21128 (18) | 0.35850 (16) | 0.20933 (11) | 0.0276 (6) | |
C5 | 0.28899 (18) | 0.30397 (16) | 0.18956 (10) | 0.0249 (6) | |
C6 | 0.34364 (18) | 0.31566 (16) | 0.13531 (11) | 0.0273 (6) | |
H6A | 0.3299 | 0.3588 | 0.1052 | 0.033* | |
C7 | 0.41838 (18) | 0.25421 (16) | 0.13462 (11) | 0.0281 (6) | |
H7A | 0.4690 | 0.2475 | 0.1049 | 0.034* | |
C8 | 0.40777 (17) | 0.20089 (16) | 0.18681 (10) | 0.0242 (6) | |
C9 | 0.46270 (18) | 0.12612 (15) | 0.19819 (10) | 0.0241 (6) | |
C10 | 0.44308 (17) | 0.07129 (15) | 0.24581 (10) | 0.0235 (6) | |
C11 | 0.48250 (18) | −0.01215 (16) | 0.25191 (11) | 0.0282 (6) | |
H11A | 0.5277 | −0.0392 | 0.2253 | 0.034* | |
C12 | 0.44379 (17) | −0.04578 (16) | 0.30252 (10) | 0.0278 (6) | |
H12A | 0.4556 | −0.1011 | 0.3174 | 0.033* | |
C13 | 0.38187 (17) | 0.01709 (15) | 0.32946 (10) | 0.0238 (6) | |
C14 | 0.33640 (17) | 0.00880 (16) | 0.38572 (10) | 0.0253 (6) | |
C15 | 0.28033 (17) | 0.07257 (16) | 0.41214 (10) | 0.0247 (6) | |
C16 | 0.24232 (18) | 0.06852 (17) | 0.47291 (11) | 0.0291 (6) | |
H16A | 0.2480 | 0.0221 | 0.5004 | 0.035* | |
C17 | 0.19734 (18) | 0.14289 (17) | 0.48343 (11) | 0.0291 (6) | |
H17A | 0.1659 | 0.1585 | 0.5199 | 0.035* | |
C18 | 0.20534 (17) | 0.19442 (17) | 0.42956 (10) | 0.0259 (6) | |
C19 | 0.16253 (17) | 0.27474 (16) | 0.42195 (11) | 0.0262 (6) | |
C20 | 0.15579 (17) | 0.31900 (16) | 0.36563 (11) | 0.0276 (6) | |
C21 | 0.17071 (19) | 0.42799 (17) | 0.16618 (11) | 0.0306 (6) | |
C22 | 0.0662 (2) | 0.4253 (2) | 0.13438 (12) | 0.0448 (8) | |
H22A | 0.0198 | 0.3793 | 0.1400 | 0.054* | |
C23 | 0.0278 (2) | 0.4896 (2) | 0.09392 (13) | 0.0549 (9) | |
H23A | −0.0449 | 0.4873 | 0.0729 | 0.066* | |
C24 | 0.0932 (3) | 0.5552 (2) | 0.08436 (13) | 0.0527 (9) | |
H24A | 0.0658 | 0.5993 | 0.0575 | 0.063* | |
C25 | 0.1991 (3) | 0.55782 (19) | 0.11349 (13) | 0.0538 (8) | |
H25A | 0.2462 | 0.6025 | 0.1056 | 0.065* | |
C26 | 0.2369 (2) | 0.49447 (18) | 0.15469 (13) | 0.0442 (8) | |
H26A | 0.3099 | 0.4970 | 0.1754 | 0.053* | |
C27 | 0.54727 (19) | 0.10185 (16) | 0.15671 (11) | 0.0287 (6) | |
C28 | 0.5185 (2) | 0.07481 (19) | 0.09618 (13) | 0.0471 (8) | |
H28A | 0.4430 | 0.0703 | 0.0802 | 0.057* | |
C29 | 0.5990 (3) | 0.0540 (2) | 0.05806 (15) | 0.0557 (9) | |
H29A | 0.5782 | 0.0362 | 0.0163 | 0.067* | |
C30 | 0.7076 (2) | 0.05926 (19) | 0.08102 (15) | 0.0496 (8) | |
H30A | 0.7625 | 0.0432 | 0.0558 | 0.059* | |
C31 | 0.7369 (2) | 0.0877 (2) | 0.14029 (15) | 0.0568 (9) | |
H31A | 0.8125 | 0.0931 | 0.1557 | 0.068* | |
C32 | 0.6575 (2) | 0.10892 (19) | 0.17839 (13) | 0.0465 (8) | |
H32A | 0.6792 | 0.1284 | 0.2197 | 0.056* | |
C33 | 0.35520 (19) | −0.07045 (16) | 0.42152 (10) | 0.0283 (6) | |
C34 | 0.4569 (2) | −0.08771 (16) | 0.45484 (11) | 0.0317 (6) | |
H34A | 0.5154 | −0.0491 | 0.4540 | 0.038* | |
C35 | 0.4745 (2) | −0.15981 (18) | 0.48913 (11) | 0.0367 (7) | |
H35A | 0.5442 | −0.1699 | 0.5124 | 0.044* | |
C36 | 0.3918 (2) | −0.21705 (18) | 0.48967 (12) | 0.0417 (7) | |
H36A | 0.4044 | −0.2676 | 0.5122 | 0.050* | |
C37 | 0.2911 (3) | −0.20076 (19) | 0.45756 (14) | 0.0550 (9) | |
H37A | 0.2334 | −0.2401 | 0.4581 | 0.066* | |
C38 | 0.2721 (2) | −0.1277 (2) | 0.42418 (13) | 0.0504 (8) | |
H38A | 0.2011 | −0.1168 | 0.4029 | 0.060* | |
C39 | 0.11998 (19) | 0.31285 (16) | 0.47754 (11) | 0.0302 (6) | |
C40 | 0.1922 (2) | 0.33033 (16) | 0.53070 (11) | 0.0339 (7) | |
H40A | 0.2689 | 0.3226 | 0.5299 | 0.041* | |
C41 | 0.1545 (2) | 0.35884 (18) | 0.58476 (12) | 0.0410 (7) | |
H41A | 0.2050 | 0.3701 | 0.6209 | 0.049* | |
C42 | 0.0436 (2) | 0.37091 (19) | 0.58608 (13) | 0.0477 (8) | |
H42A | 0.0170 | 0.3904 | 0.6231 | 0.057* | |
C43 | −0.0284 (2) | 0.3545 (2) | 0.53326 (14) | 0.0523 (9) | |
H43A | −0.1049 | 0.3634 | 0.5340 | 0.063* | |
C44 | 0.0086 (2) | 0.32529 (18) | 0.47950 (12) | 0.0411 (8) | |
H44A | −0.0423 | 0.3137 | 0.4437 | 0.049* | |
C45 | 0.4482 (2) | 0.34025 (17) | 0.37326 (11) | 0.0296 (6) | |
H45A | 0.3849 | 0.3719 | 0.3793 | 0.035* | |
C46 | 0.54733 (19) | 0.24360 (16) | 0.34800 (10) | 0.0298 (6) | |
H46A | 0.5727 | 0.1925 | 0.3328 | 0.036* | |
C47 | 0.79790 (19) | 0.44323 (18) | 0.33174 (14) | 0.0398 (7) | |
H47A | 0.7827 | 0.4792 | 0.3646 | 0.048* | |
C48 | 0.8416 (2) | 0.3978 (3) | 0.24890 (14) | 0.0554 (9) | |
H48A | 0.8653 | 0.3956 | 0.2086 | 0.067* | |
B1 | 0.7413 (2) | 0.3085 (2) | 0.38421 (15) | 0.0363 (8) | |
H1B | 0.7688 (18) | 0.3420 (16) | 0.4301 (12) | 0.047 (7)* | |
H2B | 0.7742 (16) | 0.2471 (16) | 0.3817 (10) | 0.030 (6)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0256 (2) | 0.0211 (2) | 0.0222 (2) | 0.00087 (16) | 0.00193 (14) | −0.00034 (17) |
O1 | 0.0254 (11) | 0.0331 (14) | 0.0360 (11) | 0.0005 (9) | 0.0026 (8) | −0.0064 (10) |
O1W | 0.0579 (14) | 0.0566 (18) | 0.0723 (16) | 0.0052 (12) | 0.0196 (12) | 0.0058 (14) |
N1 | 0.0255 (10) | 0.0263 (13) | 0.0230 (11) | 0.0001 (9) | 0.0022 (8) | −0.0020 (10) |
N2 | 0.0242 (10) | 0.0196 (12) | 0.0244 (11) | 0.0004 (9) | −0.0002 (8) | −0.0002 (10) |
N3 | 0.0237 (10) | 0.0244 (13) | 0.0216 (11) | −0.0028 (9) | 0.0025 (8) | 0.0006 (10) |
N4 | 0.0251 (10) | 0.0231 (13) | 0.0229 (11) | 0.0008 (9) | 0.0024 (8) | −0.0028 (10) |
N5 | 0.0277 (12) | 0.0228 (14) | 0.0269 (11) | −0.0008 (10) | −0.0005 (8) | −0.0012 (10) |
N6 | 0.0355 (13) | 0.0265 (14) | 0.0374 (13) | −0.0019 (11) | 0.0011 (10) | 0.0007 (11) |
N7 | 0.0303 (11) | 0.0277 (14) | 0.0288 (11) | −0.0042 (11) | −0.0003 (9) | 0.0052 (10) |
N8 | 0.0292 (11) | 0.0254 (14) | 0.0391 (13) | −0.0002 (10) | 0.0011 (9) | 0.0013 (11) |
N9 | 0.0521 (15) | 0.0525 (19) | 0.0398 (14) | 0.0025 (13) | 0.0064 (11) | −0.0018 (14) |
N10 | 0.0351 (13) | 0.0417 (18) | 0.0757 (19) | 0.0053 (12) | 0.0080 (12) | 0.0265 (16) |
C1 | 0.0359 (15) | 0.0322 (18) | 0.0341 (16) | 0.0099 (13) | 0.0040 (11) | −0.0080 (13) |
C2 | 0.0351 (14) | 0.0286 (18) | 0.0377 (16) | 0.0113 (12) | −0.0003 (11) | 0.0007 (13) |
C3 | 0.0265 (13) | 0.0223 (16) | 0.0323 (15) | 0.0046 (11) | −0.0010 (11) | 0.0005 (12) |
C4 | 0.0267 (13) | 0.0249 (16) | 0.0295 (15) | −0.0016 (11) | −0.0031 (11) | 0.0034 (12) |
C5 | 0.0264 (13) | 0.0222 (15) | 0.0246 (13) | −0.0014 (12) | −0.0035 (10) | 0.0013 (12) |
C6 | 0.0311 (13) | 0.0233 (16) | 0.0258 (14) | 0.0007 (12) | −0.0033 (10) | 0.0064 (12) |
C7 | 0.0291 (13) | 0.0274 (17) | 0.0285 (14) | −0.0027 (12) | 0.0056 (10) | 0.0027 (12) |
C8 | 0.0241 (13) | 0.0255 (16) | 0.0235 (13) | −0.0024 (11) | 0.0044 (10) | 0.0011 (12) |
C9 | 0.0278 (13) | 0.0226 (16) | 0.0220 (13) | −0.0016 (11) | 0.0029 (10) | 0.0008 (11) |
C10 | 0.0234 (12) | 0.0209 (15) | 0.0260 (13) | 0.0013 (11) | 0.0015 (10) | −0.0013 (12) |
C11 | 0.0310 (13) | 0.0243 (16) | 0.0300 (14) | 0.0033 (12) | 0.0068 (11) | −0.0009 (12) |
C12 | 0.0317 (14) | 0.0220 (16) | 0.0290 (14) | 0.0032 (11) | 0.0009 (11) | 0.0018 (12) |
C13 | 0.0247 (12) | 0.0209 (15) | 0.0251 (13) | 0.0005 (11) | 0.0001 (10) | 0.0013 (12) |
C14 | 0.0267 (13) | 0.0232 (16) | 0.0254 (13) | −0.0049 (11) | 0.0004 (10) | 0.0004 (12) |
C15 | 0.0277 (13) | 0.0237 (16) | 0.0223 (13) | −0.0034 (11) | 0.0009 (10) | −0.0004 (12) |
C16 | 0.0354 (14) | 0.0269 (17) | 0.0254 (14) | −0.0072 (12) | 0.0049 (11) | 0.0028 (12) |
C17 | 0.0302 (14) | 0.0338 (18) | 0.0237 (14) | −0.0043 (12) | 0.0053 (10) | −0.0056 (13) |
C18 | 0.0214 (12) | 0.0318 (17) | 0.0243 (13) | −0.0055 (12) | 0.0013 (10) | −0.0038 (13) |
C19 | 0.0228 (13) | 0.0297 (17) | 0.0256 (14) | −0.0018 (11) | 0.0005 (10) | −0.0040 (12) |
C20 | 0.0234 (13) | 0.0274 (17) | 0.0311 (14) | 0.0009 (11) | −0.0003 (10) | −0.0062 (12) |
C21 | 0.0355 (15) | 0.0292 (17) | 0.0269 (14) | 0.0081 (13) | 0.0026 (11) | 0.0010 (12) |
C22 | 0.0379 (16) | 0.058 (2) | 0.0384 (16) | 0.0069 (15) | 0.0040 (12) | 0.0135 (16) |
C23 | 0.0419 (17) | 0.079 (3) | 0.0430 (18) | 0.0218 (18) | 0.0016 (14) | 0.0156 (18) |
C24 | 0.070 (2) | 0.049 (2) | 0.0388 (17) | 0.0304 (19) | 0.0074 (16) | 0.0143 (16) |
C25 | 0.078 (2) | 0.030 (2) | 0.0524 (19) | 0.0102 (17) | 0.0016 (17) | 0.0050 (16) |
C26 | 0.0540 (18) | 0.0302 (19) | 0.0447 (17) | 0.0034 (15) | −0.0093 (14) | 0.0059 (15) |
C27 | 0.0335 (15) | 0.0216 (16) | 0.0321 (15) | 0.0019 (12) | 0.0089 (11) | 0.0100 (12) |
C28 | 0.0436 (17) | 0.048 (2) | 0.0526 (19) | −0.0046 (14) | 0.0160 (14) | −0.0164 (16) |
C29 | 0.067 (2) | 0.050 (2) | 0.056 (2) | −0.0066 (17) | 0.0297 (17) | −0.0183 (17) |
C30 | 0.054 (2) | 0.038 (2) | 0.065 (2) | 0.0049 (15) | 0.0364 (16) | 0.0053 (17) |
C31 | 0.0358 (17) | 0.072 (3) | 0.065 (2) | 0.0032 (16) | 0.0164 (15) | 0.010 (2) |
C32 | 0.0378 (17) | 0.066 (2) | 0.0379 (16) | 0.0028 (15) | 0.0120 (13) | 0.0025 (16) |
C33 | 0.0392 (15) | 0.0225 (16) | 0.0242 (13) | 0.0000 (12) | 0.0083 (11) | 0.0006 (12) |
C34 | 0.0413 (16) | 0.0259 (17) | 0.0282 (14) | 0.0004 (12) | 0.0050 (11) | 0.0002 (13) |
C35 | 0.0529 (17) | 0.0328 (19) | 0.0240 (14) | 0.0061 (15) | 0.0037 (12) | 0.0033 (13) |
C36 | 0.073 (2) | 0.0288 (18) | 0.0243 (15) | 0.0073 (16) | 0.0099 (14) | 0.0064 (13) |
C37 | 0.067 (2) | 0.037 (2) | 0.060 (2) | −0.0186 (16) | 0.0015 (16) | 0.0166 (17) |
C38 | 0.0487 (18) | 0.042 (2) | 0.057 (2) | −0.0108 (15) | −0.0076 (14) | 0.0118 (16) |
C39 | 0.0326 (14) | 0.0294 (17) | 0.0289 (14) | 0.0025 (12) | 0.0055 (11) | −0.0044 (12) |
C40 | 0.0313 (14) | 0.0317 (18) | 0.0374 (16) | 0.0041 (12) | −0.0013 (12) | −0.0063 (13) |
C41 | 0.0468 (17) | 0.041 (2) | 0.0328 (16) | 0.0086 (14) | −0.0042 (12) | −0.0132 (14) |
C42 | 0.0535 (19) | 0.053 (2) | 0.0374 (17) | 0.0099 (16) | 0.0090 (14) | −0.0166 (15) |
C43 | 0.0336 (16) | 0.070 (2) | 0.054 (2) | 0.0096 (15) | 0.0100 (14) | −0.0154 (18) |
C44 | 0.0308 (15) | 0.056 (2) | 0.0358 (16) | 0.0032 (13) | 0.0017 (12) | −0.0148 (15) |
C45 | 0.0312 (15) | 0.0278 (17) | 0.0292 (14) | −0.0005 (12) | 0.0017 (11) | 0.0045 (13) |
C46 | 0.0369 (15) | 0.0243 (17) | 0.0269 (14) | −0.0033 (13) | −0.0013 (11) | 0.0015 (12) |
C47 | 0.0311 (15) | 0.0264 (19) | 0.063 (2) | 0.0006 (13) | 0.0093 (13) | 0.0055 (16) |
C48 | 0.0465 (18) | 0.079 (3) | 0.0425 (19) | 0.0090 (18) | 0.0119 (14) | 0.023 (2) |
B1 | 0.0339 (17) | 0.034 (2) | 0.0404 (19) | −0.0063 (16) | 0.0005 (14) | 0.0102 (17) |
Geometric parameters (Å, º) top
Mn1—N4 | 2.0012 (19) | C10—C11 | 1.427 (3) |
Mn1—N3 | 2.0042 (19) | C11—C12 | 1.353 (3) |
Mn1—N2 | 2.0049 (18) | C12—C13 | 1.429 (3) |
Mn1—N1 | 2.0050 (19) | C13—C14 | 1.400 (3) |
Mn1—O1 | 2.2198 (17) | C14—C15 | 1.393 (3) |
Mn1—N5 | 2.2836 (19) | C14—C33 | 1.493 (3) |
N1—C20 | 1.384 (3) | C15—C16 | 1.443 (3) |
N1—C3 | 1.385 (3) | C16—C17 | 1.347 (3) |
N2—C5 | 1.381 (3) | C17—C18 | 1.439 (3) |
N2—C8 | 1.382 (3) | C18—C19 | 1.396 (3) |
N3—C13 | 1.383 (3) | C19—C20 | 1.400 (3) |
N3—C10 | 1.393 (3) | C19—C39 | 1.494 (3) |
N4—C15 | 1.380 (3) | C21—C22 | 1.378 (3) |
N4—C18 | 1.384 (3) | C21—C26 | 1.382 (4) |
N5—C46 | 1.330 (3) | C22—C23 | 1.396 (4) |
N5—C45 | 1.357 (3) | C23—C24 | 1.356 (4) |
N6—C45 | 1.315 (3) | C24—C25 | 1.371 (4) |
N6—N7 | 1.368 (3) | C25—C26 | 1.393 (4) |
N7—C46 | 1.333 (3) | C27—C32 | 1.379 (3) |
N7—B1 | 1.561 (3) | C27—C28 | 1.379 (3) |
N8—C47 | 1.322 (3) | C28—C29 | 1.399 (4) |
N8—N9 | 1.372 (3) | C29—C30 | 1.364 (4) |
N8—B1 | 1.540 (4) | C30—C31 | 1.363 (4) |
N9—C48 | 1.331 (4) | C31—C32 | 1.389 (4) |
N10—C47 | 1.327 (3) | C33—C38 | 1.378 (4) |
N10—C48 | 1.339 (4) | C33—C34 | 1.389 (3) |
C1—C2 | 1.348 (3) | C34—C35 | 1.378 (3) |
C1—C20 | 1.429 (3) | C35—C36 | 1.370 (4) |
C2—C3 | 1.434 (3) | C36—C37 | 1.364 (4) |
C3—C4 | 1.400 (3) | C37—C38 | 1.383 (4) |
C4—C5 | 1.398 (3) | C39—C44 | 1.385 (3) |
C4—C21 | 1.499 (3) | C39—C40 | 1.389 (3) |
C5—C6 | 1.428 (3) | C40—C41 | 1.382 (3) |
C6—C7 | 1.348 (3) | C41—C42 | 1.376 (4) |
C7—C8 | 1.432 (3) | C42—C43 | 1.378 (4) |
C8—C9 | 1.385 (3) | C43—C44 | 1.376 (3) |
C9—C10 | 1.395 (3) | B1—H2B | 1.07 (2) |
C9—C27 | 1.499 (3) | B1—H1B | 1.14 (2) |
| | | |
N4—Mn1—N3 | 89.52 (8) | N3—C13—C14 | 125.4 (2) |
N4—Mn1—N2 | 179.02 (7) | N3—C13—C12 | 109.8 (2) |
N3—Mn1—N2 | 89.87 (7) | C14—C13—C12 | 124.8 (2) |
N4—Mn1—N1 | 90.20 (8) | C15—C14—C13 | 123.4 (2) |
N3—Mn1—N1 | 178.84 (7) | C15—C14—C33 | 118.1 (2) |
N2—Mn1—N1 | 90.42 (8) | C13—C14—C33 | 118.4 (2) |
N4—Mn1—O1 | 91.25 (7) | N4—C15—C14 | 126.1 (2) |
N3—Mn1—O1 | 90.75 (7) | N4—C15—C16 | 109.3 (2) |
N2—Mn1—O1 | 89.53 (7) | C14—C15—C16 | 124.5 (2) |
N1—Mn1—O1 | 88.13 (7) | C17—C16—C15 | 107.2 (2) |
N4—Mn1—N5 | 92.00 (7) | C16—C17—C18 | 107.9 (2) |
N3—Mn1—N5 | 92.27 (7) | N4—C18—C19 | 126.4 (2) |
N2—Mn1—N5 | 87.26 (7) | N4—C18—C17 | 109.0 (2) |
N1—Mn1—N5 | 88.87 (7) | C19—C18—C17 | 124.5 (2) |
O1—Mn1—N5 | 175.59 (7) | C18—C19—C20 | 123.6 (2) |
C20—N1—C3 | 106.2 (2) | C18—C19—C39 | 116.6 (2) |
C20—N1—Mn1 | 127.09 (16) | C20—C19—C39 | 119.7 (2) |
C3—N1—Mn1 | 126.65 (15) | N1—C20—C19 | 125.2 (2) |
C5—N2—C8 | 106.30 (19) | N1—C20—C1 | 109.2 (2) |
C5—N2—Mn1 | 126.90 (15) | C19—C20—C1 | 125.6 (2) |
C8—N2—Mn1 | 126.54 (15) | C22—C21—C26 | 117.7 (2) |
C13—N3—C10 | 105.73 (19) | C22—C21—C4 | 120.2 (2) |
C13—N3—Mn1 | 127.21 (15) | C26—C21—C4 | 122.0 (2) |
C10—N3—Mn1 | 126.82 (16) | C21—C22—C23 | 120.6 (3) |
C15—N4—C18 | 106.55 (19) | C24—C23—C22 | 120.7 (3) |
C15—N4—Mn1 | 127.23 (15) | C23—C24—C25 | 119.9 (3) |
C18—N4—Mn1 | 126.20 (17) | C24—C25—C26 | 119.5 (3) |
C46—N5—C45 | 101.75 (19) | C21—C26—C25 | 121.5 (3) |
C46—N5—Mn1 | 128.15 (17) | C32—C27—C28 | 118.3 (2) |
C45—N5—Mn1 | 129.23 (15) | C32—C27—C9 | 119.7 (2) |
C45—N6—N7 | 103.4 (2) | C28—C27—C9 | 121.9 (2) |
C46—N7—N6 | 108.00 (19) | C27—C28—C29 | 120.8 (3) |
C46—N7—B1 | 130.2 (2) | C30—C29—C28 | 119.9 (3) |
N6—N7—B1 | 121.7 (2) | C31—C30—C29 | 119.7 (3) |
C47—N8—N9 | 108.1 (2) | C30—C31—C32 | 120.8 (3) |
C47—N8—B1 | 128.2 (3) | C27—C32—C31 | 120.4 (3) |
N9—N8—B1 | 123.6 (2) | C38—C33—C34 | 117.8 (2) |
C48—N9—N8 | 101.9 (3) | C38—C33—C14 | 121.5 (2) |
C47—N10—C48 | 101.0 (3) | C34—C33—C14 | 120.7 (2) |
C2—C1—C20 | 107.9 (2) | C35—C34—C33 | 121.2 (2) |
C1—C2—C3 | 107.3 (2) | C36—C35—C34 | 120.1 (2) |
N1—C3—C4 | 125.6 (2) | C37—C36—C35 | 119.4 (3) |
N1—C3—C2 | 109.3 (2) | C36—C37—C38 | 120.8 (3) |
C4—C3—C2 | 124.7 (2) | C33—C38—C37 | 120.7 (3) |
C5—C4—C3 | 124.0 (2) | C44—C39—C40 | 118.5 (2) |
C5—C4—C21 | 117.7 (2) | C44—C39—C19 | 121.6 (2) |
C3—C4—C21 | 118.2 (2) | C40—C39—C19 | 119.7 (2) |
N2—C5—C4 | 125.6 (2) | C41—C40—C39 | 121.2 (2) |
N2—C5—C6 | 109.5 (2) | C42—C41—C40 | 119.7 (2) |
C4—C5—C6 | 124.8 (2) | C41—C42—C43 | 119.4 (3) |
C7—C6—C5 | 107.4 (2) | C44—C43—C42 | 121.1 (2) |
C6—C7—C8 | 107.7 (2) | C43—C44—C39 | 120.1 (2) |
N2—C8—C9 | 126.0 (2) | N6—C45—N5 | 114.9 (2) |
N2—C8—C7 | 109.0 (2) | N5—C46—N7 | 111.9 (2) |
C9—C8—C7 | 124.8 (2) | N8—C47—N10 | 112.9 (3) |
C8—C9—C10 | 123.7 (2) | N9—C48—N10 | 116.1 (3) |
C8—C9—C27 | 118.4 (2) | H2B—B1—H1B | 113.9 (17) |
C10—C9—C27 | 117.8 (2) | H2B—B1—N8 | 107.9 (12) |
N3—C10—C9 | 125.4 (2) | H1B—B1—N8 | 105.2 (13) |
N3—C10—C11 | 109.4 (2) | H2B—B1—N7 | 109.4 (12) |
C9—C10—C11 | 125.1 (2) | H1B—B1—N7 | 111.0 (12) |
C12—C11—C10 | 107.6 (2) | N8—B1—N7 | 109.2 (2) |
C11—C12—C13 | 107.4 (2) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H2O···O1W | 0.84 (2) | 1.97 (1) | 2.804 (3) | 175 (2) |
O1—H1O···N10i | 0.84 (2) | 1.90 (1) | 2.728 (3) | 169 (3) |
O1W—H2W···N9ii | 0.84 (2) | 2.12 (1) | 2.945 (3) | 166 (3) |
O1W—H1W···Cg1iii | 0.84 (2) | 2.90 (3) | 3.673 (3) | 154 (3) |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) x−1, y, z; (iii) −x, y−1/2, −z+1/2. |