Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
Two novel polymers exhibiting metal–organic frameworks (MOFs) have been synthesized by the combination of a metal ion with a benzene-1,3,5-tri­carboxyl­ate ligand (BTC) and 1,10-phenanthroline (phen) under hydro­thermal conditions. The first compound, poly[[(μ4-benzene-1,3,5-tri­carboxyl­ato-κ4O:O′:O′′:O′′′)(μ-hydroxido-κ2O:O)bis­(1,10-phenanthroline-κ2N,N′)dizinc(II)] 0.32-hydrate], {[Zn2(C9H3O6)(OH)(C12H8N2)2]·0.32H2O}n, denoted Zn–MOF, forms a two-dimensional network in which a binuclear Zn2 cluster serves as a 3-connecting node; the BTC trianion also acts as a 3-connecting centre. The overall topology is that of a 63 net. The phen ligands serve as appendages to the network and inter­digitate with phen ligands belonging to adjacent parallel sheets. The second compound, poly[[­(μ6-benzene-1,3,5-tri­carboxyl­ato-κ7O1,O1′:O1:O3:O3′:O5:O5′)­(μ3-hydroxido-κ2O:O:O)(1,10-phenanthroline-κ2N,N′)di­manganese(II)] 1.26-hydrate], {[Mn2(C9H3O6)(OH)(C12H8N2)]·1.26H2O}n, denoted Mn–MOF, exists as a three-dimensional network in which an Mn4 cluster serves as a 6-connecting unit, while the BTC trianion again plays the role of a 3-connecting centre. The overall topology is that of the rutile net. Phen ligands act as appendages to the network and form the `S-shaped' packing mode.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614005828/wq3051sup1.cif
Contains datablocks global, HUT-13, HUT-14

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614005828/wq3051HUT-13sup2.hkl
Contains datablock hut-13

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614005828/wq3051HUT-14sup3.hkl
Contains datablock zr099b

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229614005828/wq3051sup4.pdf
Supplementary material

CCDC references: 991883; 991884

Computing details top

Data collection: CrystalClear-SM Expert (Rigaku, 2009) for HUT-13; CrysAlis PRO (Oxford Diffraction, 2010) for HUT-14. Cell refinement: CrystalClear-SM Expert (Rigaku, 2009) for HUT-13; CrysAlis PRO (Oxford Diffraction, 2010) for HUT-14. Data reduction: CrystalClear-SM Expert (Rigaku, 2009) for HUT-13; CrysAlis PRO (Oxford Diffraction, 2010) for HUT-14. For both structures, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: WinGX (Farrugia, 2012); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Poly[[(µ4-benzene-1,3,5-tricarboxylato-κ4O:O':O'':O''')(µ-hydroxido-κ2O:O')bis(1,10-phenanthroline-κ2N,N')dizinc(II)] monohydrate] (HUT-13) top
Crystal data top
[Zn2(C9H3O6)(OH)(C12H8N2)2]·0.32H2OF(000) = 1464
Mr = 723.27Dx = 1.671 Mg m3
Monoclinic, P21/nSynchrotron radiation, λ = 0.6889 Å
Hall symbol: -P 2ynCell parameters from 10993 reflections
a = 11.9003 (1) Åθ = 1.8–29.5°
b = 17.6185 (3) ŵ = 1.59 mm1
c = 13.7173 (2) ÅT = 100 K
β = 91.157 (1)°Prism, colourless
V = 2875.46 (7) Å30.1 × 0.05 × 0.03 mm
Z = 4
Data collection top
Dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images
diffractometer
5228 reflections with I > 2σ(I)
Synchrotron monochromatorRint = 0.037
ω scansθmax = 25.5°, θmin = 5.0°
Absorption correction: multi-scan
(CrysAlis PRO; Oxford Diffraction, 2010)
h = 1414
Tmin = 0.568, Tmax = 1k = 2222
23044 measured reflectionsl = 1317
5681 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.134H atoms treated by a mixture of independent and constrained refinement
S = 1.21 w = 1/[σ2(Fo2) + (0.062P)2 + 4.8591P]
where P = (Fo2 + 2Fc2)/3
5681 reflections(Δ/σ)max = 0.001
429 parametersΔρmax = 0.76 e Å3
0 restraintsΔρmin = 0.49 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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
xyzUiso*/UeqOcc. (<1)
Zn10.76234 (3)0.34704 (2)0.67610 (3)0.01928 (13)
Zn20.76462 (3)0.343444 (19)0.91459 (3)0.01930 (13)
N20.5908 (2)0.39526 (15)0.9175 (2)0.0239 (6)
N30.5822 (2)0.39791 (16)0.6597 (2)0.0265 (6)
N40.7878 (2)0.46036 (16)0.6362 (2)0.0262 (6)
N10.7940 (2)0.46096 (15)0.8973 (2)0.0231 (6)
O10.7158 (2)0.28990 (13)0.79240 (18)0.0224 (5)
H500.644 (4)0.287 (2)0.796 (3)0.029 (10)*
O20.9284 (2)0.33818 (13)0.72358 (19)0.0257 (5)
O30.93052 (18)0.32019 (14)0.88727 (17)0.0242 (5)
O40.7386 (2)0.28113 (13)0.03337 (17)0.0245 (5)
O50.7465 (2)0.28737 (14)0.55590 (18)0.0255 (5)
O60.8990 (3)0.3293 (2)0.4789 (2)0.0491 (8)
O70.8292 (2)0.37397 (16)0.1124 (2)0.0378 (7)
C10.8947 (3)0.4940 (2)0.8948 (3)0.0336 (8)
H10.95950.46380.90760.040*
C20.9094 (3)0.5717 (2)0.8738 (3)0.0423 (10)
H20.98250.59350.87450.051*
C30.8167 (3)0.6152 (2)0.8523 (3)0.0393 (9)
H30.82530.66730.83620.047*
C40.7084 (3)0.5827 (2)0.8541 (3)0.0320 (8)
C50.7016 (3)0.50485 (18)0.8796 (2)0.0242 (7)
C60.6063 (3)0.6239 (2)0.8339 (3)0.0356 (9)
H60.61040.67550.81440.043*
C70.5053 (3)0.5908 (2)0.8422 (3)0.0357 (9)
H70.43940.61960.82830.043*
C80.4942 (3)0.5123 (2)0.8718 (3)0.0300 (8)
C90.5928 (3)0.46906 (19)0.8892 (3)0.0255 (7)
C100.3903 (3)0.4755 (2)0.8864 (3)0.0359 (9)
H100.32180.50240.87620.043*
C110.3887 (3)0.4011 (2)0.9152 (3)0.0359 (9)
H110.31930.37590.92550.043*
C120.4910 (3)0.3625 (2)0.9293 (3)0.0313 (8)
H120.48900.31060.94820.038*
C130.8891 (3)0.4893 (2)0.6205 (3)0.0344 (8)
H130.95310.45800.63140.041*
C140.9054 (4)0.5646 (2)0.5883 (3)0.0413 (10)
H140.97900.58310.57720.050*
C150.8133 (4)0.6107 (2)0.5733 (3)0.0404 (9)
H150.82290.66160.55200.049*
C160.7043 (3)0.5819 (2)0.5898 (3)0.0329 (8)
C170.6958 (3)0.50536 (19)0.6195 (3)0.0283 (7)
C180.6028 (4)0.6259 (2)0.5751 (3)0.0396 (9)
H180.60820.67750.55560.048*
C190.5009 (4)0.5949 (2)0.5887 (3)0.0397 (9)
H190.43570.62530.57870.048*
C200.4884 (3)0.5167 (2)0.6181 (3)0.0346 (8)
C210.5862 (3)0.4720 (2)0.6334 (3)0.0280 (7)
C220.3836 (3)0.4815 (3)0.6323 (3)0.0406 (9)
H220.31600.50960.62380.049*
C230.3799 (3)0.4062 (2)0.6584 (3)0.0388 (9)
H230.31000.38160.66820.047*
C240.4815 (3)0.3664 (2)0.6705 (3)0.0336 (8)
H240.47810.31420.68720.040*
C310.5898 (2)0.21746 (17)0.2991 (2)0.0205 (6)
C320.6468 (3)0.23587 (17)0.3856 (2)0.0211 (6)
H320.61650.22080.44610.025*
C330.7481 (3)0.27617 (18)0.3847 (3)0.0224 (7)
C340.7902 (3)0.29957 (18)0.2941 (2)0.0221 (7)
H340.85740.32860.29240.027*
C350.7348 (2)0.28076 (18)0.2073 (2)0.0217 (7)
C360.6352 (3)0.23770 (17)0.2092 (2)0.0214 (6)
H360.59900.22250.15010.026*
C370.9735 (3)0.31716 (18)0.8033 (2)0.0220 (7)
C380.8046 (3)0.30024 (19)0.4794 (3)0.0270 (7)
C390.7732 (3)0.31423 (19)0.1114 (3)0.0240 (7)
OW10.1444 (10)0.5005 (9)0.7536 (13)0.089 (7)0.316 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0181 (2)0.0219 (2)0.0178 (2)0.00046 (13)0.00019 (16)0.00089 (13)
Zn20.0183 (2)0.0220 (2)0.0178 (2)0.00187 (13)0.00397 (16)0.00098 (13)
N20.0235 (14)0.0242 (13)0.0241 (16)0.0007 (11)0.0062 (12)0.0015 (11)
N30.0250 (14)0.0287 (14)0.0259 (16)0.0017 (11)0.0004 (12)0.0033 (12)
N40.0256 (14)0.0250 (14)0.0280 (17)0.0016 (11)0.0004 (13)0.0008 (12)
N10.0211 (13)0.0255 (14)0.0229 (15)0.0000 (11)0.0031 (12)0.0011 (11)
O10.0214 (12)0.0256 (11)0.0204 (13)0.0013 (9)0.0026 (10)0.0000 (9)
O20.0169 (11)0.0380 (13)0.0222 (14)0.0040 (9)0.0007 (10)0.0062 (10)
O30.0175 (11)0.0340 (12)0.0212 (13)0.0060 (9)0.0028 (10)0.0013 (10)
O40.0288 (12)0.0279 (12)0.0169 (12)0.0012 (9)0.0033 (10)0.0019 (9)
O50.0254 (12)0.0334 (13)0.0178 (12)0.0068 (10)0.0012 (10)0.0021 (10)
O60.0354 (16)0.081 (2)0.0309 (17)0.0322 (15)0.0040 (13)0.0067 (15)
O70.0401 (15)0.0451 (15)0.0284 (15)0.0187 (12)0.0052 (12)0.0035 (12)
C10.0237 (17)0.0363 (19)0.041 (2)0.0012 (14)0.0041 (16)0.0015 (16)
C20.0323 (19)0.0337 (19)0.061 (3)0.0100 (16)0.0127 (19)0.0042 (18)
C30.044 (2)0.0277 (18)0.047 (3)0.0057 (16)0.0132 (19)0.0009 (16)
C40.0366 (19)0.0265 (17)0.033 (2)0.0025 (14)0.0084 (16)0.0009 (14)
C50.0251 (16)0.0251 (15)0.0226 (17)0.0014 (12)0.0044 (14)0.0001 (13)
C60.045 (2)0.0262 (17)0.036 (2)0.0083 (15)0.0045 (18)0.0019 (15)
C70.036 (2)0.0340 (19)0.037 (2)0.0122 (15)0.0029 (17)0.0030 (16)
C80.0264 (18)0.0318 (17)0.032 (2)0.0059 (14)0.0017 (15)0.0054 (14)
C90.0252 (16)0.0278 (16)0.0237 (18)0.0026 (13)0.0044 (14)0.0036 (13)
C100.0234 (17)0.044 (2)0.041 (2)0.0063 (15)0.0022 (16)0.0095 (17)
C110.0262 (18)0.042 (2)0.039 (2)0.0057 (15)0.0067 (16)0.0115 (17)
C120.0301 (18)0.0303 (17)0.034 (2)0.0036 (14)0.0090 (16)0.0051 (15)
C130.0295 (18)0.0338 (19)0.040 (2)0.0050 (14)0.0017 (17)0.0054 (16)
C140.041 (2)0.038 (2)0.045 (3)0.0125 (17)0.0000 (19)0.0069 (18)
C150.055 (2)0.0288 (18)0.037 (2)0.0067 (17)0.0013 (19)0.0036 (16)
C160.044 (2)0.0284 (17)0.0263 (19)0.0016 (15)0.0037 (16)0.0004 (14)
C170.0337 (18)0.0274 (16)0.0236 (18)0.0015 (14)0.0011 (15)0.0008 (13)
C180.058 (3)0.0265 (18)0.034 (2)0.0101 (17)0.0009 (19)0.0033 (15)
C190.049 (2)0.035 (2)0.036 (2)0.0175 (17)0.0023 (19)0.0017 (16)
C200.0333 (19)0.0374 (19)0.033 (2)0.0099 (15)0.0014 (17)0.0006 (15)
C210.0290 (17)0.0319 (17)0.0230 (18)0.0053 (14)0.0011 (14)0.0016 (14)
C220.0291 (19)0.055 (2)0.038 (2)0.0125 (17)0.0019 (17)0.0024 (18)
C230.0258 (18)0.054 (2)0.037 (2)0.0005 (16)0.0024 (16)0.0002 (18)
C240.0308 (19)0.0390 (19)0.031 (2)0.0007 (15)0.0009 (16)0.0025 (16)
C310.0172 (14)0.0206 (14)0.0237 (17)0.0013 (11)0.0025 (13)0.0014 (12)
C320.0188 (14)0.0230 (14)0.0217 (17)0.0011 (11)0.0035 (13)0.0014 (12)
C330.0192 (15)0.0255 (15)0.0225 (17)0.0018 (12)0.0020 (13)0.0003 (12)
C340.0188 (14)0.0260 (15)0.0217 (17)0.0021 (12)0.0025 (13)0.0000 (12)
C350.0195 (15)0.0247 (15)0.0211 (17)0.0031 (11)0.0039 (13)0.0004 (12)
C360.0198 (15)0.0245 (15)0.0200 (16)0.0039 (12)0.0004 (13)0.0007 (12)
C370.0196 (15)0.0237 (15)0.0229 (17)0.0004 (12)0.0023 (13)0.0006 (12)
C380.0231 (16)0.0322 (17)0.0257 (19)0.0065 (13)0.0014 (14)0.0019 (14)
C390.0186 (15)0.0288 (16)0.0248 (18)0.0017 (12)0.0047 (13)0.0036 (13)
OW10.048 (8)0.091 (11)0.128 (15)0.003 (6)0.010 (8)0.043 (9)
Geometric parameters (Å, º) top
Zn1—O51.961 (2)C5—C91.448 (5)
Zn1—O11.975 (2)C6—C71.343 (6)
Zn1—O22.074 (2)C7—C81.447 (5)
Zn1—N42.094 (3)C8—C101.414 (5)
Zn1—N32.330 (3)C8—C91.416 (5)
Zn2—O4i1.994 (2)C10—C111.370 (6)
Zn2—O12.000 (2)C11—C121.405 (5)
Zn2—O32.058 (2)C13—C141.413 (5)
Zn2—N12.114 (3)C14—C151.377 (6)
Zn2—N22.262 (3)C15—C161.416 (6)
N2—C121.334 (4)C16—C171.412 (5)
N2—C91.357 (4)C16—C181.445 (6)
N3—C241.332 (5)C17—C211.448 (5)
N3—C211.355 (4)C18—C191.346 (6)
N4—C131.330 (4)C19—C201.444 (6)
N4—C171.368 (5)C20—C221.410 (6)
N1—C11.333 (4)C20—C211.418 (5)
N1—C51.363 (4)C22—C231.375 (6)
O2—C371.264 (4)C23—C241.404 (5)
O3—C371.271 (4)C31—C321.393 (5)
O4—C391.280 (4)C31—C361.402 (4)
O4—Zn2ii1.994 (2)C31—C37iii1.514 (4)
O5—C381.288 (4)C32—C331.399 (4)
O6—C381.235 (4)C33—C341.411 (4)
O7—C391.246 (4)C33—C381.512 (5)
C1—C21.410 (5)C34—C351.389 (5)
C2—C31.372 (6)C35—C361.408 (4)
C3—C41.411 (5)C35—C391.520 (4)
C4—C51.417 (5)C37—C31iv1.514 (4)
C4—C61.438 (5)
O5—Zn1—O1112.46 (10)C10—C8—C7124.2 (3)
O5—Zn1—O2107.35 (10)C9—C8—C7118.8 (3)
O1—Zn1—O289.39 (10)N2—C9—C8123.0 (3)
O5—Zn1—N4107.67 (11)N2—C9—C5117.6 (3)
O1—Zn1—N4137.85 (11)C8—C9—C5119.3 (3)
O2—Zn1—N490.66 (11)C11—C10—C8119.8 (3)
O5—Zn1—N393.03 (11)C10—C11—C12119.1 (3)
O1—Zn1—N390.07 (10)N2—C12—C11123.0 (3)
O2—Zn1—N3158.13 (10)N4—C13—C14122.8 (4)
N4—Zn1—N375.28 (11)C15—C14—C13119.2 (4)
O4i—Zn2—O1112.20 (10)C14—C15—C16119.6 (4)
O4i—Zn2—O3101.81 (10)C17—C16—C15117.3 (4)
O1—Zn2—O390.99 (10)C17—C16—C18119.2 (4)
O4i—Zn2—N1131.26 (11)C15—C16—C18123.4 (4)
O1—Zn2—N1114.47 (11)N4—C17—C16122.7 (3)
O3—Zn2—N190.75 (10)N4—C17—C21117.6 (3)
O4i—Zn2—N292.91 (10)C16—C17—C21119.7 (3)
O1—Zn2—N287.39 (10)C19—C18—C16121.0 (3)
O3—Zn2—N2164.66 (10)C18—C19—C20121.6 (4)
N1—Zn2—N276.12 (10)C22—C20—C21117.4 (4)
C12—N2—C9118.1 (3)C22—C20—C19123.7 (4)
C12—N2—Zn2130.1 (2)C21—C20—C19118.9 (4)
C9—N2—Zn2111.1 (2)N3—C21—C20122.8 (3)
C24—N3—C21117.8 (3)N3—C21—C17117.6 (3)
C24—N3—Zn1131.1 (2)C20—C21—C17119.6 (3)
C21—N3—Zn1111.1 (2)C23—C22—C20119.6 (4)
C13—N4—C17118.4 (3)C22—C23—C24118.7 (4)
C13—N4—Zn1123.0 (2)N3—C24—C23123.6 (4)
C17—N4—Zn1118.5 (2)C32—C31—C36120.0 (3)
C1—N1—C5118.1 (3)C32—C31—C37iii119.5 (3)
C1—N1—Zn2125.5 (2)C36—C31—C37iii120.3 (3)
C5—N1—Zn2116.2 (2)C31—C32—C33121.1 (3)
Zn1—O1—Zn2110.79 (11)C32—C33—C34118.5 (3)
C37—O2—Zn1132.7 (2)C32—C33—C38120.2 (3)
C37—O3—Zn2125.4 (2)C34—C33—C38121.0 (3)
C39—O4—Zn2ii112.3 (2)C35—C34—C33120.9 (3)
C38—O5—Zn1123.1 (2)C34—C35—C36119.8 (3)
N1—C1—C2123.0 (3)C34—C35—C39120.2 (3)
C3—C2—C1119.0 (3)C36—C35—C39119.5 (3)
C2—C3—C4120.0 (3)C31—C36—C35119.6 (3)
C3—C4—C5117.1 (3)O2—C37—O3126.9 (3)
C3—C4—C6124.0 (3)O2—C37—C31iv117.2 (3)
C5—C4—C6118.9 (3)O3—C37—C31iv115.9 (3)
N1—C5—C4122.9 (3)O6—C38—O5125.5 (3)
N1—C5—C9117.2 (3)O6—C38—C33120.0 (3)
C4—C5—C9120.0 (3)O5—C38—C33114.5 (3)
C7—C6—C4121.3 (3)O7—C39—O4123.8 (3)
C6—C7—C8121.7 (3)O7—C39—C35119.3 (3)
C10—C8—C9117.0 (3)O4—C39—C35116.7 (3)
Symmetry codes: (i) x, y, z+1; (ii) x, y, z1; (iii) x1/2, y+1/2, z1/2; (iv) x+1/2, y+1/2, z+1/2.
Poly[[bis(µ6-benzene-1,3,5-tricarboxylato-κ4O:O':O'':O''')bis(µ3-hydroxido-κ2O:O:O)bis(µ2-hydroxido-κ2O:O)bis(1,10-phenanthroline-κ2N,N')tetramanganese(II)] 1.32-hydrate] (HUT-14) top
Crystal data top
[Mn2(C9H3O6)(OH)(C12H8N2)]·1.26H2OF(000) = 1056
Mr = 528.29Dx = 1.739 Mg m3
Monoclinic, P21/nCu Kα radiation, λ = 1.54184 Å
Hall symbol: -P 2ynCell parameters from 16326 reflections
a = 10.0433 (1) Åθ = 4.1–76.1°
b = 10.8307 (1) ŵ = 10.71 mm1
c = 18.5159 (1) ÅT = 150 K
β = 93.779 (1)°Block, yellow
V = 2009.71 (3) Å30.10 × 0.08 × 0.03 mm
Z = 4
Data collection top
Oxford SuperNova Dual
diffractometer (Cu at zero) with an Atlas detector
3807 independent reflections
Graphite monochromator3540 reflections with I > 2σ(I)
Detector resolution: 10.4102 pixels mm-1Rint = 0.040
ω scansθmax = 70.1°, θmin = 6.0°
Absorption correction: multi-scan
(CrysAlis PRO; Oxford Diffraction, 2010)
h = 1212
Tmin = 0.703, Tmax = 1k = 1313
32065 measured reflectionsl = 2222
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.077H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0373P)2 + 1.574P]
where P = (Fo2 + 2Fc2)/3
3807 reflections(Δ/σ)max = 0.001
283 parametersΔρmax = 0.56 e Å3
39 restraintsΔρmin = 0.38 e Å3
Special details top

Experimental. Absorption correction: CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.38 (release 10-08-2010 CrysAlis171 .NET) (compiled Aug 10 2010,17:59:35) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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
xyzUiso*/UeqOcc. (<1)
Mn10.27665 (3)0.82104 (3)0.524677 (17)0.02440 (10)
Mn20.46630 (3)1.01549 (3)0.410433 (16)0.02304 (10)
O10.47220 (13)0.87375 (14)0.49193 (7)0.0247 (3)
H10.53250.80280.48260.03*
O20.54482 (15)0.81213 (16)0.64935 (9)0.0351 (4)
O30.35623 (18)0.71283 (19)0.61295 (9)0.0451 (5)
O40.68861 (15)0.54367 (16)0.94854 (8)0.0328 (4)
O50.79427 (15)0.54255 (17)0.84685 (9)0.0359 (4)
O60.19497 (16)0.48099 (19)0.90574 (9)0.0411 (4)
O70.08759 (15)0.60227 (19)0.82919 (10)0.0457 (5)
C10.4498 (2)0.67468 (19)0.73041 (11)0.0234 (4)
C20.56871 (19)0.64562 (19)0.77022 (11)0.0230 (4)
H20.6520.66270.75080.028*
C30.56516 (19)0.59171 (19)0.83819 (11)0.0217 (4)
C40.44334 (19)0.56856 (19)0.86725 (11)0.0232 (4)
H40.44110.53560.91470.028*
C50.32478 (19)0.5938 (2)0.82666 (11)0.0238 (4)
C60.32878 (19)0.6470 (2)0.75863 (11)0.0252 (4)
H60.24780.66470.73110.03*
C70.4513 (2)0.7382 (2)0.65822 (11)0.0283 (4)
C80.6920 (2)0.55701 (19)0.88113 (12)0.0253 (4)
C90.1947 (2)0.5585 (2)0.85525 (11)0.0274 (4)
N1A0.2393 (6)0.6862 (5)0.4348 (3)0.0291 (15)*0.449 (6)
N2A0.0695 (6)0.7451 (7)0.5380 (4)0.032 (2)*0.449 (6)
C10A0.0577 (7)0.5782 (6)0.3652 (3)0.0377 (15)*0.449 (6)
C11A0.0233 (6)0.6747 (5)0.4796 (4)0.0272 (15)*0.449 (6)
C12A0.1105 (7)0.6459 (5)0.4254 (3)0.0251 (14)*0.449 (6)
C13A0.1634 (7)0.5671 (5)0.4126 (4)0.0345 (14)*0.449 (6)
H13A0.2540.54140.40780.041*0.449 (6)
C14A0.1122 (6)0.6356 (6)0.4744 (4)0.0395 (16)*0.449 (6)
C15A0.0763 (8)0.5396 (7)0.3600 (4)0.0516 (18)*0.449 (6)
H15A0.1080.49290.3190.062*0.449 (6)
C16A0.0138 (7)0.7710 (6)0.5898 (4)0.0376 (17)*0.449 (6)
H16A0.02090.81830.630.045*0.449 (6)
C17A0.3201 (8)0.6609 (6)0.3827 (3)0.0425 (16)*0.449 (6)
H17A0.40970.68930.38760.051*0.449 (6)
C18A0.1495 (7)0.7337 (6)0.5896 (5)0.0412 (15)*0.449 (6)
H18A0.20510.75320.62760.049*0.449 (6)
C19A0.2769 (9)0.5935 (7)0.3207 (4)0.0487 (18)*0.449 (6)
H19A0.33670.57530.28450.058*0.449 (6)
C20A0.1456 (9)0.5541 (5)0.3135 (3)0.0353 (14)*0.449 (6)
H20A0.11560.5090.27150.042*0.449 (6)
C21A0.1932 (7)0.6671 (7)0.5296 (5)0.0456 (16)*0.449 (6)
H21A0.28370.64110.52550.055*0.449 (6)
N1B0.2037 (6)0.6767 (4)0.4373 (2)0.0291 (12)*0.551 (6)
N2B0.0703 (5)0.7492 (5)0.5524 (3)0.0295 (16)*0.551 (6)
C10B0.0089 (6)0.5842 (4)0.3793 (3)0.0365 (12)*0.551 (6)
C11B0.0008 (5)0.6872 (4)0.4984 (3)0.0242 (11)*0.551 (6)
C12B0.0719 (6)0.6498 (4)0.4382 (3)0.0259 (11)*0.551 (6)
C13B0.1973 (6)0.5896 (5)0.4399 (4)0.0479 (14)*0.551 (6)
H13B0.28960.57020.43990.057*0.551 (6)
C14B0.1347 (5)0.6545 (4)0.4991 (3)0.0323 (11)*0.551 (6)
C15B0.1255 (6)0.5540 (5)0.3821 (3)0.0374 (12)*0.551 (6)
H15B0.16870.50820.34350.045*0.551 (6)
C16B0.0088 (5)0.7760 (5)0.6106 (3)0.0343 (13)*0.551 (6)
H16B0.0580.81440.65010.041*0.551 (6)
C17B0.2729 (6)0.6438 (5)0.3809 (3)0.0357 (12)*0.551 (6)
H17B0.36470.66560.38180.043*0.551 (6)
C18B0.1270 (5)0.7503 (5)0.6171 (4)0.0421 (13)*0.551 (6)
H18B0.16970.77270.65940.05*0.551 (6)
C19B0.2168 (7)0.5783 (5)0.3196 (3)0.0361 (11)*0.551 (6)
H19B0.26830.55540.28050.043*0.551 (6)
C20B0.0828 (7)0.5499 (5)0.3205 (3)0.0433 (13)*0.551 (6)
H20B0.03990.50660.28090.052*0.551 (6)
C21B0.1971 (5)0.6912 (5)0.5597 (4)0.0398 (12)*0.551 (6)
H21B0.28970.67580.56240.048*0.551 (6)
O1W0.5470 (8)0.6539 (8)0.2833 (5)0.124 (4)*0.523 (10)
O2W0000.18 (2)*0.21 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.02117 (16)0.03535 (19)0.01631 (16)0.00438 (13)0.00138 (11)0.00062 (13)
Mn20.01591 (15)0.03624 (19)0.01676 (16)0.00384 (12)0.00053 (11)0.00365 (13)
O10.0210 (7)0.0338 (8)0.0194 (7)0.0030 (6)0.0029 (5)0.0027 (6)
O20.0254 (7)0.0472 (10)0.0321 (8)0.0084 (7)0.0035 (6)0.0183 (7)
O30.0415 (9)0.0621 (12)0.0293 (9)0.0217 (9)0.0150 (7)0.0203 (8)
O40.0333 (8)0.0407 (9)0.0228 (8)0.0065 (7)0.0099 (6)0.0059 (7)
O50.0206 (7)0.0543 (10)0.0319 (8)0.0090 (7)0.0051 (6)0.0015 (8)
O60.0298 (8)0.0604 (12)0.0336 (9)0.0025 (8)0.0054 (7)0.0232 (8)
O70.0200 (8)0.0656 (12)0.0518 (11)0.0037 (8)0.0044 (7)0.0240 (10)
C10.0219 (9)0.0275 (10)0.0206 (10)0.0032 (8)0.0004 (7)0.0045 (8)
C20.0172 (9)0.0293 (10)0.0224 (10)0.0019 (7)0.0007 (7)0.0015 (8)
C30.0185 (9)0.0252 (10)0.0207 (9)0.0003 (7)0.0031 (7)0.0003 (8)
C40.0232 (9)0.0271 (10)0.0190 (9)0.0001 (8)0.0012 (7)0.0032 (8)
C50.0194 (9)0.0293 (10)0.0225 (10)0.0014 (8)0.0004 (7)0.0032 (8)
C60.0183 (9)0.0320 (11)0.0248 (10)0.0003 (8)0.0034 (7)0.0059 (8)
C70.0232 (10)0.0378 (12)0.0234 (10)0.0026 (9)0.0017 (8)0.0084 (9)
C80.0217 (9)0.0261 (10)0.0270 (11)0.0017 (8)0.0070 (8)0.0004 (8)
C90.0225 (10)0.0377 (12)0.0222 (10)0.0023 (9)0.0022 (8)0.0029 (9)
Geometric parameters (Å, º) top
Mn1—O32.1241 (17)C5—C61.388 (3)
Mn1—O6i2.1665 (18)C5—C91.491 (3)
Mn1—O12.1697 (14)N1A—C17A1.329 (8)
Mn1—O4ii2.1799 (16)N1A—C12A1.365 (8)
Mn1—N1A2.227 (5)N2A—C16A1.343 (8)
Mn1—N2A2.266 (6)N2A—C11A1.378 (9)
Mn1—N2B2.303 (5)C10A—C20A1.369 (9)
Mn1—N1B2.332 (4)C10A—C15A1.406 (9)
Mn2—O5ii2.1209 (15)C10A—C12A1.408 (7)
Mn2—O12.1508 (15)C11A—C12A1.410 (8)
Mn2—O2iii2.1696 (16)C11A—C14A1.423 (7)
Mn2—O1iii2.2229 (15)C13A—C15A1.384 (9)
Mn2—O6iv2.3043 (16)C13A—C14A1.430 (9)
Mn2—O7iv2.3695 (17)C14A—C21A1.390 (9)
O1—Mn2iii2.2229 (15)C16A—C18A1.422 (9)
O2—C71.253 (3)C17A—C19A1.405 (9)
O2—Mn2iii2.1696 (16)C18A—C21A1.373 (10)
O3—C71.259 (3)C19A—C20A1.385 (9)
O4—C81.259 (3)N1B—C17B1.342 (6)
O4—Mn1v2.1799 (16)N1B—C12B1.356 (7)
O5—C81.253 (3)N2B—C16B1.311 (7)
O5—Mn2v2.1209 (15)N2B—C11B1.358 (7)
O6—C91.257 (3)C10B—C15B1.392 (8)
O6—Mn1vi2.1665 (17)C10B—C20B1.407 (7)
O6—Mn2vii2.3043 (16)C10B—C12B1.415 (6)
O7—C91.244 (3)C11B—C14B1.408 (6)
O7—Mn2vii2.3695 (17)C11B—C12B1.422 (7)
C1—C61.387 (3)C13B—C15B1.386 (7)
C1—C21.397 (3)C13B—C14B1.413 (7)
C1—C71.504 (3)C14B—C21B1.380 (8)
C2—C31.390 (3)C16B—C18B1.404 (7)
C3—C41.391 (3)C17B—C19B1.422 (7)
C3—C81.504 (3)C18B—C21B1.391 (8)
C4—C51.393 (3)C19B—C20B1.382 (7)
O3—Mn1—O6i87.45 (8)C4—C5—C9119.74 (18)
O3—Mn1—O193.36 (6)C1—C6—C5120.65 (18)
O6i—Mn1—O182.52 (6)O2—C7—O3126.5 (2)
O3—Mn1—O4ii169.92 (7)O2—C7—C1117.41 (18)
O6i—Mn1—O4ii83.05 (7)O3—C7—C1116.11 (19)
O1—Mn1—O4ii88.77 (6)O5—C8—O4124.36 (19)
O3—Mn1—N1A104.44 (15)O5—C8—C3117.24 (19)
O6i—Mn1—N1A167.89 (15)O4—C8—C3118.40 (19)
O1—Mn1—N1A94.30 (17)O7—C9—O6120.2 (2)
O4ii—Mn1—N1A85.21 (14)O7—C9—C5121.4 (2)
O3—Mn1—N2A90.99 (19)O6—C9—C5118.45 (19)
O6i—Mn1—N2A108.13 (18)C17A—N1A—C12A117.4 (6)
O1—Mn1—N2A168.68 (18)C17A—N1A—Mn1126.6 (5)
O4ii—Mn1—N2A88.77 (19)C12A—N1A—Mn1114.7 (4)
N1A—Mn1—N2A74.5 (2)C16A—N2A—C11A118.9 (6)
O3—Mn1—N2B86.60 (15)C16A—N2A—Mn1128.4 (5)
O6i—Mn1—N2B102.88 (15)C11A—N2A—Mn1112.3 (5)
O1—Mn1—N2B174.59 (15)C20A—C10A—C15A123.6 (6)
O4ii—Mn1—N2B92.21 (15)C20A—C10A—C12A115.2 (6)
N1A—Mn1—N2B80.5 (2)C15A—C10A—C12A121.2 (7)
N2A—Mn1—N2B6.7 (2)N2A—C11A—C12A119.3 (5)
O3—Mn1—N1B104.40 (12)N2A—C11A—C14A119.3 (7)
O6i—Mn1—N1B166.24 (12)C12A—C11A—C14A121.4 (6)
O1—Mn1—N1B103.39 (14)N1A—C12A—C10A124.9 (6)
O4ii—Mn1—N1B84.64 (11)N1A—C12A—C11A117.7 (5)
N1A—Mn1—N1B9.13 (16)C10A—C12A—C11A117.4 (6)
N2A—Mn1—N1B65.4 (2)C15A—C13A—C14A117.6 (6)
N2B—Mn1—N1B71.42 (19)C21A—C14A—C11A118.7 (6)
O5ii—Mn2—O199.30 (6)C21A—C14A—C13A121.2 (6)
O5ii—Mn2—O2iii87.66 (7)C11A—C14A—C13A120.1 (7)
O1—Mn2—O2iii166.01 (6)C13A—C15A—C10A122.3 (6)
O5ii—Mn2—O1iii141.62 (6)N2A—C16A—C18A125.5 (7)
O1—Mn2—O1iii79.70 (6)N1A—C17A—C19A122.0 (7)
O2iii—Mn2—O1iii87.29 (6)C21A—C18A—C16A114.0 (6)
O5ii—Mn2—O6iv139.59 (6)C20A—C19A—C17A118.7 (7)
O1—Mn2—O6iv93.26 (6)C10A—C20A—C19A121.8 (6)
O2iii—Mn2—O6iv89.11 (7)C18A—C21A—C14A123.6 (6)
O1iii—Mn2—O6iv78.32 (5)C17B—N1B—C12B120.5 (5)
O5ii—Mn2—O7iv85.53 (6)C17B—N1B—Mn1124.2 (4)
O1—Mn2—O7iv93.99 (7)C12B—N1B—Mn1113.5 (3)
O2iii—Mn2—O7iv98.66 (7)C16B—N2B—C11B117.9 (5)
O1iii—Mn2—O7iv132.83 (5)C16B—N2B—Mn1126.0 (4)
O6iv—Mn2—O7iv55.22 (6)C11B—N2B—Mn1115.4 (4)
Mn2—O1—Mn1113.60 (6)C15B—C10B—C20B121.9 (5)
Mn2—O1—Mn2iii100.30 (6)C15B—C10B—C12B118.3 (6)
Mn1—O1—Mn2iii97.06 (5)C20B—C10B—C12B119.7 (5)
C7—O2—Mn2iii127.09 (14)N2B—C11B—C14B124.6 (5)
C7—O3—Mn1128.50 (16)N2B—C11B—C12B117.3 (4)
C8—O4—Mn1v121.85 (14)C14B—C11B—C12B118.1 (5)
C8—O5—Mn2v114.91 (14)N1B—C12B—C10B119.1 (6)
C9—O6—Mn1vi166.07 (17)N1B—C12B—C11B119.2 (4)
C9—O6—Mn2vii93.67 (13)C10B—C12B—C11B121.7 (5)
Mn1vi—O6—Mn2vii94.77 (6)C15B—C13B—C14B120.6 (5)
C9—O7—Mn2vii90.95 (14)C21B—C14B—C11B115.2 (5)
C6—C1—C2119.50 (19)C21B—C14B—C13B124.8 (5)
C6—C1—C7119.60 (18)C11B—C14B—C13B120.0 (6)
C2—C1—C7120.88 (18)C13B—C15B—C10B121.2 (5)
C3—C2—C1120.01 (18)N2B—C16B—C18B122.6 (6)
C2—C3—C4120.10 (18)N1B—C17B—C19B123.7 (6)
C2—C3—C8120.81 (18)C21B—C18B—C16B118.1 (5)
C4—C3—C8119.08 (18)C20B—C19B—C17B115.9 (5)
C3—C4—C5119.88 (18)C19B—C20B—C10B121.0 (5)
C6—C5—C4119.76 (18)C14B—C21B—C18B121.3 (5)
C6—C5—C9120.46 (18)
Symmetry codes: (i) x+1/2, y+1/2, z+3/2; (ii) x1/2, y+3/2, z1/2; (iii) x+1, y+2, z+1; (iv) x+1/2, y+3/2, z1/2; (v) x+1/2, y+3/2, z+1/2; (vi) x+1/2, y1/2, z+3/2; (vii) x1/2, y+3/2, z+1/2.
 

Subscribe to Acta Crystallographica Section C: Structural Chemistry

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds