Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614005828/wq3051sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614005828/wq3051HUT-13sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614005828/wq3051HUT-14sup3.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229614005828/wq3051sup4.pdf |
CCDC references: 991883; 991884
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).
[Zn2(C9H3O6)(OH)(C12H8N2)2]·0.32H2O | F(000) = 1464 |
Mr = 723.27 | Dx = 1.671 Mg m−3 |
Monoclinic, P21/n | Synchrotron radiation, λ = 0.6889 Å |
Hall symbol: -P 2yn | Cell parameters from 10993 reflections |
a = 11.9003 (1) Å | θ = 1.8–29.5° |
b = 17.6185 (3) Å | µ = 1.59 mm−1 |
c = 13.7173 (2) Å | T = 100 K |
β = 91.157 (1)° | Prism, colourless |
V = 2875.46 (7) Å3 | 0.1 × 0.05 × 0.03 mm |
Z = 4 |
Dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images diffractometer | 5228 reflections with I > 2σ(I) |
Synchrotron monochromator | Rint = 0.037 |
ω scans | θmax = 25.5°, θmin = 5.0° |
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010) | h = −14→14 |
Tmin = 0.568, Tmax = 1 | k = −22→22 |
23044 measured reflections | l = −13→17 |
5681 independent reflections |
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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.134 | H 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 parameters | Δρmax = 0.76 e Å−3 |
0 restraints | Δρmin = −0.49 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn1 | 0.76234 (3) | 0.34704 (2) | 0.67610 (3) | 0.01928 (13) | |
Zn2 | 0.76462 (3) | 0.343444 (19) | 0.91459 (3) | 0.01930 (13) | |
N2 | 0.5908 (2) | 0.39526 (15) | 0.9175 (2) | 0.0239 (6) | |
N3 | 0.5822 (2) | 0.39791 (16) | 0.6597 (2) | 0.0265 (6) | |
N4 | 0.7878 (2) | 0.46036 (16) | 0.6362 (2) | 0.0262 (6) | |
N1 | 0.7940 (2) | 0.46096 (15) | 0.8973 (2) | 0.0231 (6) | |
O1 | 0.7158 (2) | 0.28990 (13) | 0.79240 (18) | 0.0224 (5) | |
H50 | 0.644 (4) | 0.287 (2) | 0.796 (3) | 0.029 (10)* | |
O2 | 0.9284 (2) | 0.33818 (13) | 0.72358 (19) | 0.0257 (5) | |
O3 | 0.93052 (18) | 0.32019 (14) | 0.88727 (17) | 0.0242 (5) | |
O4 | 0.7386 (2) | 0.28113 (13) | 0.03337 (17) | 0.0245 (5) | |
O5 | 0.7465 (2) | 0.28737 (14) | 0.55590 (18) | 0.0255 (5) | |
O6 | 0.8990 (3) | 0.3293 (2) | 0.4789 (2) | 0.0491 (8) | |
O7 | 0.8292 (2) | 0.37397 (16) | 0.1124 (2) | 0.0378 (7) | |
C1 | 0.8947 (3) | 0.4940 (2) | 0.8948 (3) | 0.0336 (8) | |
H1 | 0.9595 | 0.4638 | 0.9076 | 0.040* | |
C2 | 0.9094 (3) | 0.5717 (2) | 0.8738 (3) | 0.0423 (10) | |
H2 | 0.9825 | 0.5935 | 0.8745 | 0.051* | |
C3 | 0.8167 (3) | 0.6152 (2) | 0.8523 (3) | 0.0393 (9) | |
H3 | 0.8253 | 0.6673 | 0.8362 | 0.047* | |
C4 | 0.7084 (3) | 0.5827 (2) | 0.8541 (3) | 0.0320 (8) | |
C5 | 0.7016 (3) | 0.50485 (18) | 0.8796 (2) | 0.0242 (7) | |
C6 | 0.6063 (3) | 0.6239 (2) | 0.8339 (3) | 0.0356 (9) | |
H6 | 0.6104 | 0.6755 | 0.8144 | 0.043* | |
C7 | 0.5053 (3) | 0.5908 (2) | 0.8422 (3) | 0.0357 (9) | |
H7 | 0.4394 | 0.6196 | 0.8283 | 0.043* | |
C8 | 0.4942 (3) | 0.5123 (2) | 0.8718 (3) | 0.0300 (8) | |
C9 | 0.5928 (3) | 0.46906 (19) | 0.8892 (3) | 0.0255 (7) | |
C10 | 0.3903 (3) | 0.4755 (2) | 0.8864 (3) | 0.0359 (9) | |
H10 | 0.3218 | 0.5024 | 0.8762 | 0.043* | |
C11 | 0.3887 (3) | 0.4011 (2) | 0.9152 (3) | 0.0359 (9) | |
H11 | 0.3193 | 0.3759 | 0.9255 | 0.043* | |
C12 | 0.4910 (3) | 0.3625 (2) | 0.9293 (3) | 0.0313 (8) | |
H12 | 0.4890 | 0.3106 | 0.9482 | 0.038* | |
C13 | 0.8891 (3) | 0.4893 (2) | 0.6205 (3) | 0.0344 (8) | |
H13 | 0.9531 | 0.4580 | 0.6314 | 0.041* | |
C14 | 0.9054 (4) | 0.5646 (2) | 0.5883 (3) | 0.0413 (10) | |
H14 | 0.9790 | 0.5831 | 0.5772 | 0.050* | |
C15 | 0.8133 (4) | 0.6107 (2) | 0.5733 (3) | 0.0404 (9) | |
H15 | 0.8229 | 0.6616 | 0.5520 | 0.049* | |
C16 | 0.7043 (3) | 0.5819 (2) | 0.5898 (3) | 0.0329 (8) | |
C17 | 0.6958 (3) | 0.50536 (19) | 0.6195 (3) | 0.0283 (7) | |
C18 | 0.6028 (4) | 0.6259 (2) | 0.5751 (3) | 0.0396 (9) | |
H18 | 0.6082 | 0.6775 | 0.5556 | 0.048* | |
C19 | 0.5009 (4) | 0.5949 (2) | 0.5887 (3) | 0.0397 (9) | |
H19 | 0.4357 | 0.6253 | 0.5787 | 0.048* | |
C20 | 0.4884 (3) | 0.5167 (2) | 0.6181 (3) | 0.0346 (8) | |
C21 | 0.5862 (3) | 0.4720 (2) | 0.6334 (3) | 0.0280 (7) | |
C22 | 0.3836 (3) | 0.4815 (3) | 0.6323 (3) | 0.0406 (9) | |
H22 | 0.3160 | 0.5096 | 0.6238 | 0.049* | |
C23 | 0.3799 (3) | 0.4062 (2) | 0.6584 (3) | 0.0388 (9) | |
H23 | 0.3100 | 0.3816 | 0.6682 | 0.047* | |
C24 | 0.4815 (3) | 0.3664 (2) | 0.6705 (3) | 0.0336 (8) | |
H24 | 0.4781 | 0.3142 | 0.6872 | 0.040* | |
C31 | 0.5898 (2) | 0.21746 (17) | 0.2991 (2) | 0.0205 (6) | |
C32 | 0.6468 (3) | 0.23587 (17) | 0.3856 (2) | 0.0211 (6) | |
H32 | 0.6165 | 0.2208 | 0.4461 | 0.025* | |
C33 | 0.7481 (3) | 0.27617 (18) | 0.3847 (3) | 0.0224 (7) | |
C34 | 0.7902 (3) | 0.29957 (18) | 0.2941 (2) | 0.0221 (7) | |
H34 | 0.8574 | 0.3286 | 0.2924 | 0.027* | |
C35 | 0.7348 (2) | 0.28076 (18) | 0.2073 (2) | 0.0217 (7) | |
C36 | 0.6352 (3) | 0.23770 (17) | 0.2092 (2) | 0.0214 (6) | |
H36 | 0.5990 | 0.2225 | 0.1501 | 0.026* | |
C37 | 0.9735 (3) | 0.31716 (18) | 0.8033 (2) | 0.0220 (7) | |
C38 | 0.8046 (3) | 0.30024 (19) | 0.4794 (3) | 0.0270 (7) | |
C39 | 0.7732 (3) | 0.31423 (19) | 0.1114 (3) | 0.0240 (7) | |
OW1 | 0.1444 (10) | 0.5005 (9) | 0.7536 (13) | 0.089 (7) | 0.316 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0181 (2) | 0.0219 (2) | 0.0178 (2) | 0.00046 (13) | −0.00019 (16) | 0.00089 (13) |
Zn2 | 0.0183 (2) | 0.0220 (2) | 0.0178 (2) | 0.00187 (13) | 0.00397 (16) | 0.00098 (13) |
N2 | 0.0235 (14) | 0.0242 (13) | 0.0241 (16) | 0.0007 (11) | 0.0062 (12) | −0.0015 (11) |
N3 | 0.0250 (14) | 0.0287 (14) | 0.0259 (16) | 0.0017 (11) | 0.0004 (12) | 0.0033 (12) |
N4 | 0.0256 (14) | 0.0250 (14) | 0.0280 (17) | −0.0016 (11) | −0.0004 (13) | 0.0008 (12) |
N1 | 0.0211 (13) | 0.0255 (14) | 0.0229 (15) | 0.0000 (11) | 0.0031 (12) | −0.0011 (11) |
O1 | 0.0214 (12) | 0.0256 (11) | 0.0204 (13) | −0.0013 (9) | 0.0026 (10) | 0.0000 (9) |
O2 | 0.0169 (11) | 0.0380 (13) | 0.0222 (14) | 0.0040 (9) | 0.0007 (10) | 0.0062 (10) |
O3 | 0.0175 (11) | 0.0340 (12) | 0.0212 (13) | 0.0060 (9) | 0.0028 (10) | −0.0013 (10) |
O4 | 0.0288 (12) | 0.0279 (12) | 0.0169 (12) | −0.0012 (9) | 0.0033 (10) | 0.0019 (9) |
O5 | 0.0254 (12) | 0.0334 (13) | 0.0178 (12) | −0.0068 (10) | 0.0012 (10) | −0.0021 (10) |
O6 | 0.0354 (16) | 0.081 (2) | 0.0309 (17) | −0.0322 (15) | 0.0040 (13) | −0.0067 (15) |
O7 | 0.0401 (15) | 0.0451 (15) | 0.0284 (15) | −0.0187 (12) | 0.0052 (12) | 0.0035 (12) |
C1 | 0.0237 (17) | 0.0363 (19) | 0.041 (2) | −0.0012 (14) | 0.0041 (16) | −0.0015 (16) |
C2 | 0.0323 (19) | 0.0337 (19) | 0.061 (3) | −0.0100 (16) | 0.0127 (19) | −0.0042 (18) |
C3 | 0.044 (2) | 0.0277 (18) | 0.047 (3) | −0.0057 (16) | 0.0132 (19) | −0.0009 (16) |
C4 | 0.0366 (19) | 0.0265 (17) | 0.033 (2) | 0.0025 (14) | 0.0084 (16) | −0.0009 (14) |
C5 | 0.0251 (16) | 0.0251 (15) | 0.0226 (17) | 0.0014 (12) | 0.0044 (14) | −0.0001 (13) |
C6 | 0.045 (2) | 0.0262 (17) | 0.036 (2) | 0.0083 (15) | 0.0045 (18) | 0.0019 (15) |
C7 | 0.036 (2) | 0.0340 (19) | 0.037 (2) | 0.0122 (15) | −0.0029 (17) | −0.0030 (16) |
C8 | 0.0264 (18) | 0.0318 (17) | 0.032 (2) | 0.0059 (14) | 0.0017 (15) | −0.0054 (14) |
C9 | 0.0252 (16) | 0.0278 (16) | 0.0237 (18) | 0.0026 (13) | 0.0044 (14) | −0.0036 (13) |
C10 | 0.0234 (17) | 0.044 (2) | 0.041 (2) | 0.0063 (15) | 0.0022 (16) | −0.0095 (17) |
C11 | 0.0262 (18) | 0.042 (2) | 0.039 (2) | −0.0057 (15) | 0.0067 (16) | −0.0115 (17) |
C12 | 0.0301 (18) | 0.0303 (17) | 0.034 (2) | −0.0036 (14) | 0.0090 (16) | −0.0051 (15) |
C13 | 0.0295 (18) | 0.0338 (19) | 0.040 (2) | −0.0050 (14) | −0.0017 (17) | 0.0054 (16) |
C14 | 0.041 (2) | 0.038 (2) | 0.045 (3) | −0.0125 (17) | 0.0000 (19) | 0.0069 (18) |
C15 | 0.055 (2) | 0.0288 (18) | 0.037 (2) | −0.0067 (17) | −0.0013 (19) | 0.0036 (16) |
C16 | 0.044 (2) | 0.0284 (17) | 0.0263 (19) | 0.0016 (15) | −0.0037 (16) | −0.0004 (14) |
C17 | 0.0337 (18) | 0.0274 (16) | 0.0236 (18) | 0.0015 (14) | −0.0011 (15) | 0.0008 (13) |
C18 | 0.058 (3) | 0.0265 (18) | 0.034 (2) | 0.0101 (17) | −0.0009 (19) | 0.0033 (15) |
C19 | 0.049 (2) | 0.035 (2) | 0.036 (2) | 0.0175 (17) | −0.0023 (19) | −0.0017 (16) |
C20 | 0.0333 (19) | 0.0374 (19) | 0.033 (2) | 0.0099 (15) | 0.0014 (17) | −0.0006 (15) |
C21 | 0.0290 (17) | 0.0319 (17) | 0.0230 (18) | 0.0053 (14) | −0.0011 (14) | −0.0016 (14) |
C22 | 0.0291 (19) | 0.055 (2) | 0.038 (2) | 0.0125 (17) | 0.0019 (17) | −0.0024 (18) |
C23 | 0.0258 (18) | 0.054 (2) | 0.037 (2) | 0.0005 (16) | 0.0024 (16) | 0.0002 (18) |
C24 | 0.0308 (19) | 0.0390 (19) | 0.031 (2) | −0.0007 (15) | 0.0009 (16) | 0.0025 (16) |
C31 | 0.0172 (14) | 0.0206 (14) | 0.0237 (17) | 0.0013 (11) | 0.0025 (13) | −0.0014 (12) |
C32 | 0.0188 (14) | 0.0230 (14) | 0.0217 (17) | 0.0011 (11) | 0.0035 (13) | 0.0014 (12) |
C33 | 0.0192 (15) | 0.0255 (15) | 0.0225 (17) | 0.0018 (12) | 0.0020 (13) | −0.0003 (12) |
C34 | 0.0188 (14) | 0.0260 (15) | 0.0217 (17) | −0.0021 (12) | 0.0025 (13) | 0.0000 (12) |
C35 | 0.0195 (15) | 0.0247 (15) | 0.0211 (17) | 0.0031 (11) | 0.0039 (13) | 0.0004 (12) |
C36 | 0.0198 (15) | 0.0245 (15) | 0.0200 (16) | 0.0039 (12) | 0.0004 (13) | −0.0007 (12) |
C37 | 0.0196 (15) | 0.0237 (15) | 0.0229 (17) | −0.0004 (12) | 0.0023 (13) | 0.0006 (12) |
C38 | 0.0231 (16) | 0.0322 (17) | 0.0257 (19) | −0.0065 (13) | 0.0014 (14) | −0.0019 (14) |
C39 | 0.0186 (15) | 0.0288 (16) | 0.0248 (18) | 0.0017 (12) | 0.0047 (13) | 0.0036 (13) |
OW1 | 0.048 (8) | 0.091 (11) | 0.128 (15) | 0.003 (6) | 0.010 (8) | −0.043 (9) |
Zn1—O5 | 1.961 (2) | C5—C9 | 1.448 (5) |
Zn1—O1 | 1.975 (2) | C6—C7 | 1.343 (6) |
Zn1—O2 | 2.074 (2) | C7—C8 | 1.447 (5) |
Zn1—N4 | 2.094 (3) | C8—C10 | 1.414 (5) |
Zn1—N3 | 2.330 (3) | C8—C9 | 1.416 (5) |
Zn2—O4i | 1.994 (2) | C10—C11 | 1.370 (6) |
Zn2—O1 | 2.000 (2) | C11—C12 | 1.405 (5) |
Zn2—O3 | 2.058 (2) | C13—C14 | 1.413 (5) |
Zn2—N1 | 2.114 (3) | C14—C15 | 1.377 (6) |
Zn2—N2 | 2.262 (3) | C15—C16 | 1.416 (6) |
N2—C12 | 1.334 (4) | C16—C17 | 1.412 (5) |
N2—C9 | 1.357 (4) | C16—C18 | 1.445 (6) |
N3—C24 | 1.332 (5) | C17—C21 | 1.448 (5) |
N3—C21 | 1.355 (4) | C18—C19 | 1.346 (6) |
N4—C13 | 1.330 (4) | C19—C20 | 1.444 (6) |
N4—C17 | 1.368 (5) | C20—C22 | 1.410 (6) |
N1—C1 | 1.333 (4) | C20—C21 | 1.418 (5) |
N1—C5 | 1.363 (4) | C22—C23 | 1.375 (6) |
O2—C37 | 1.264 (4) | C23—C24 | 1.404 (5) |
O3—C37 | 1.271 (4) | C31—C32 | 1.393 (5) |
O4—C39 | 1.280 (4) | C31—C36 | 1.402 (4) |
O4—Zn2ii | 1.994 (2) | C31—C37iii | 1.514 (4) |
O5—C38 | 1.288 (4) | C32—C33 | 1.399 (4) |
O6—C38 | 1.235 (4) | C33—C34 | 1.411 (4) |
O7—C39 | 1.246 (4) | C33—C38 | 1.512 (5) |
C1—C2 | 1.410 (5) | C34—C35 | 1.389 (5) |
C2—C3 | 1.372 (6) | C35—C36 | 1.408 (4) |
C3—C4 | 1.411 (5) | C35—C39 | 1.520 (4) |
C4—C5 | 1.417 (5) | C37—C31iv | 1.514 (4) |
C4—C6 | 1.438 (5) | ||
O5—Zn1—O1 | 112.46 (10) | C10—C8—C7 | 124.2 (3) |
O5—Zn1—O2 | 107.35 (10) | C9—C8—C7 | 118.8 (3) |
O1—Zn1—O2 | 89.39 (10) | N2—C9—C8 | 123.0 (3) |
O5—Zn1—N4 | 107.67 (11) | N2—C9—C5 | 117.6 (3) |
O1—Zn1—N4 | 137.85 (11) | C8—C9—C5 | 119.3 (3) |
O2—Zn1—N4 | 90.66 (11) | C11—C10—C8 | 119.8 (3) |
O5—Zn1—N3 | 93.03 (11) | C10—C11—C12 | 119.1 (3) |
O1—Zn1—N3 | 90.07 (10) | N2—C12—C11 | 123.0 (3) |
O2—Zn1—N3 | 158.13 (10) | N4—C13—C14 | 122.8 (4) |
N4—Zn1—N3 | 75.28 (11) | C15—C14—C13 | 119.2 (4) |
O4i—Zn2—O1 | 112.20 (10) | C14—C15—C16 | 119.6 (4) |
O4i—Zn2—O3 | 101.81 (10) | C17—C16—C15 | 117.3 (4) |
O1—Zn2—O3 | 90.99 (10) | C17—C16—C18 | 119.2 (4) |
O4i—Zn2—N1 | 131.26 (11) | C15—C16—C18 | 123.4 (4) |
O1—Zn2—N1 | 114.47 (11) | N4—C17—C16 | 122.7 (3) |
O3—Zn2—N1 | 90.75 (10) | N4—C17—C21 | 117.6 (3) |
O4i—Zn2—N2 | 92.91 (10) | C16—C17—C21 | 119.7 (3) |
O1—Zn2—N2 | 87.39 (10) | C19—C18—C16 | 121.0 (3) |
O3—Zn2—N2 | 164.66 (10) | C18—C19—C20 | 121.6 (4) |
N1—Zn2—N2 | 76.12 (10) | C22—C20—C21 | 117.4 (4) |
C12—N2—C9 | 118.1 (3) | C22—C20—C19 | 123.7 (4) |
C12—N2—Zn2 | 130.1 (2) | C21—C20—C19 | 118.9 (4) |
C9—N2—Zn2 | 111.1 (2) | N3—C21—C20 | 122.8 (3) |
C24—N3—C21 | 117.8 (3) | N3—C21—C17 | 117.6 (3) |
C24—N3—Zn1 | 131.1 (2) | C20—C21—C17 | 119.6 (3) |
C21—N3—Zn1 | 111.1 (2) | C23—C22—C20 | 119.6 (4) |
C13—N4—C17 | 118.4 (3) | C22—C23—C24 | 118.7 (4) |
C13—N4—Zn1 | 123.0 (2) | N3—C24—C23 | 123.6 (4) |
C17—N4—Zn1 | 118.5 (2) | C32—C31—C36 | 120.0 (3) |
C1—N1—C5 | 118.1 (3) | C32—C31—C37iii | 119.5 (3) |
C1—N1—Zn2 | 125.5 (2) | C36—C31—C37iii | 120.3 (3) |
C5—N1—Zn2 | 116.2 (2) | C31—C32—C33 | 121.1 (3) |
Zn1—O1—Zn2 | 110.79 (11) | C32—C33—C34 | 118.5 (3) |
C37—O2—Zn1 | 132.7 (2) | C32—C33—C38 | 120.2 (3) |
C37—O3—Zn2 | 125.4 (2) | C34—C33—C38 | 121.0 (3) |
C39—O4—Zn2ii | 112.3 (2) | C35—C34—C33 | 120.9 (3) |
C38—O5—Zn1 | 123.1 (2) | C34—C35—C36 | 119.8 (3) |
N1—C1—C2 | 123.0 (3) | C34—C35—C39 | 120.2 (3) |
C3—C2—C1 | 119.0 (3) | C36—C35—C39 | 119.5 (3) |
C2—C3—C4 | 120.0 (3) | C31—C36—C35 | 119.6 (3) |
C3—C4—C5 | 117.1 (3) | O2—C37—O3 | 126.9 (3) |
C3—C4—C6 | 124.0 (3) | O2—C37—C31iv | 117.2 (3) |
C5—C4—C6 | 118.9 (3) | O3—C37—C31iv | 115.9 (3) |
N1—C5—C4 | 122.9 (3) | O6—C38—O5 | 125.5 (3) |
N1—C5—C9 | 117.2 (3) | O6—C38—C33 | 120.0 (3) |
C4—C5—C9 | 120.0 (3) | O5—C38—C33 | 114.5 (3) |
C7—C6—C4 | 121.3 (3) | O7—C39—O4 | 123.8 (3) |
C6—C7—C8 | 121.7 (3) | O7—C39—C35 | 119.3 (3) |
C10—C8—C9 | 117.0 (3) | O4—C39—C35 | 116.7 (3) |
Symmetry codes: (i) x, y, z+1; (ii) x, y, z−1; (iii) x−1/2, −y+1/2, z−1/2; (iv) x+1/2, −y+1/2, z+1/2. |
[Mn2(C9H3O6)(OH)(C12H8N2)]·1.26H2O | F(000) = 1056 |
Mr = 528.29 | Dx = 1.739 Mg m−3 |
Monoclinic, P21/n | Cu Kα radiation, λ = 1.54184 Å |
Hall symbol: -P 2yn | Cell parameters from 16326 reflections |
a = 10.0433 (1) Å | θ = 4.1–76.1° |
b = 10.8307 (1) Å | µ = 10.71 mm−1 |
c = 18.5159 (1) Å | T = 150 K |
β = 93.779 (1)° | Block, yellow |
V = 2009.71 (3) Å3 | 0.10 × 0.08 × 0.03 mm |
Z = 4 |
Oxford SuperNova Dual diffractometer (Cu at zero) with an Atlas detector | 3807 independent reflections |
Graphite monochromator | 3540 reflections with I > 2σ(I) |
Detector resolution: 10.4102 pixels mm-1 | Rint = 0.040 |
ω scans | θmax = 70.1°, θmin = 6.0° |
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010) | h = −12→12 |
Tmin = 0.703, Tmax = 1 | k = −13→13 |
32065 measured reflections | l = −22→22 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.077 | H-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 parameters | Δρmax = 0.56 e Å−3 |
39 restraints | Δρmin = −0.38 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Mn1 | 0.27665 (3) | 0.82104 (3) | 0.524677 (17) | 0.02440 (10) | |
Mn2 | 0.46630 (3) | 1.01549 (3) | 0.410433 (16) | 0.02304 (10) | |
O1 | 0.47220 (13) | 0.87375 (14) | 0.49193 (7) | 0.0247 (3) | |
H1 | 0.5325 | 0.8028 | 0.4826 | 0.03* | |
O2 | 0.54482 (15) | 0.81213 (16) | 0.64935 (9) | 0.0351 (4) | |
O3 | 0.35623 (18) | 0.71283 (19) | 0.61295 (9) | 0.0451 (5) | |
O4 | 0.68861 (15) | 0.54367 (16) | 0.94854 (8) | 0.0328 (4) | |
O5 | 0.79427 (15) | 0.54255 (17) | 0.84685 (9) | 0.0359 (4) | |
O6 | 0.19497 (16) | 0.48099 (19) | 0.90574 (9) | 0.0411 (4) | |
O7 | 0.08759 (15) | 0.60227 (19) | 0.82919 (10) | 0.0457 (5) | |
C1 | 0.4498 (2) | 0.67468 (19) | 0.73041 (11) | 0.0234 (4) | |
C2 | 0.56871 (19) | 0.64562 (19) | 0.77022 (11) | 0.0230 (4) | |
H2 | 0.652 | 0.6627 | 0.7508 | 0.028* | |
C3 | 0.56516 (19) | 0.59171 (19) | 0.83819 (11) | 0.0217 (4) | |
C4 | 0.44334 (19) | 0.56856 (19) | 0.86725 (11) | 0.0232 (4) | |
H4 | 0.4411 | 0.5356 | 0.9147 | 0.028* | |
C5 | 0.32478 (19) | 0.5938 (2) | 0.82666 (11) | 0.0238 (4) | |
C6 | 0.32878 (19) | 0.6470 (2) | 0.75863 (11) | 0.0252 (4) | |
H6 | 0.2478 | 0.6647 | 0.7311 | 0.03* | |
C7 | 0.4513 (2) | 0.7382 (2) | 0.65822 (11) | 0.0283 (4) | |
C8 | 0.6920 (2) | 0.55701 (19) | 0.88113 (12) | 0.0253 (4) | |
C9 | 0.1947 (2) | 0.5585 (2) | 0.85525 (11) | 0.0274 (4) | |
N1A | 0.2393 (6) | 0.6862 (5) | 0.4348 (3) | 0.0291 (15)* | 0.449 (6) |
N2A | 0.0695 (6) | 0.7451 (7) | 0.5380 (4) | 0.032 (2)* | 0.449 (6) |
C10A | 0.0577 (7) | 0.5782 (6) | 0.3652 (3) | 0.0377 (15)* | 0.449 (6) |
C11A | 0.0233 (6) | 0.6747 (5) | 0.4796 (4) | 0.0272 (15)* | 0.449 (6) |
C12A | 0.1105 (7) | 0.6459 (5) | 0.4254 (3) | 0.0251 (14)* | 0.449 (6) |
C13A | −0.1634 (7) | 0.5671 (5) | 0.4126 (4) | 0.0345 (14)* | 0.449 (6) |
H13A | −0.254 | 0.5414 | 0.4078 | 0.041* | 0.449 (6) |
C14A | −0.1122 (6) | 0.6356 (6) | 0.4744 (4) | 0.0395 (16)* | 0.449 (6) |
C15A | −0.0763 (8) | 0.5396 (7) | 0.3600 (4) | 0.0516 (18)* | 0.449 (6) |
H15A | −0.108 | 0.4929 | 0.319 | 0.062* | 0.449 (6) |
C16A | −0.0138 (7) | 0.7710 (6) | 0.5898 (4) | 0.0376 (17)* | 0.449 (6) |
H16A | 0.0209 | 0.8183 | 0.63 | 0.045* | 0.449 (6) |
C17A | 0.3201 (8) | 0.6609 (6) | 0.3827 (3) | 0.0425 (16)* | 0.449 (6) |
H17A | 0.4097 | 0.6893 | 0.3876 | 0.051* | 0.449 (6) |
C18A | −0.1495 (7) | 0.7337 (6) | 0.5896 (5) | 0.0412 (15)* | 0.449 (6) |
H18A | −0.2051 | 0.7532 | 0.6276 | 0.049* | 0.449 (6) |
C19A | 0.2769 (9) | 0.5935 (7) | 0.3207 (4) | 0.0487 (18)* | 0.449 (6) |
H19A | 0.3367 | 0.5753 | 0.2845 | 0.058* | 0.449 (6) |
C20A | 0.1456 (9) | 0.5541 (5) | 0.3135 (3) | 0.0353 (14)* | 0.449 (6) |
H20A | 0.1156 | 0.509 | 0.2715 | 0.042* | 0.449 (6) |
C21A | −0.1932 (7) | 0.6671 (7) | 0.5296 (5) | 0.0456 (16)* | 0.449 (6) |
H21A | −0.2837 | 0.6411 | 0.5255 | 0.055* | 0.449 (6) |
N1B | 0.2037 (6) | 0.6767 (4) | 0.4373 (2) | 0.0291 (12)* | 0.551 (6) |
N2B | 0.0703 (5) | 0.7492 (5) | 0.5524 (3) | 0.0295 (16)* | 0.551 (6) |
C10B | 0.0089 (6) | 0.5842 (4) | 0.3793 (3) | 0.0365 (12)* | 0.551 (6) |
C11B | 0.0008 (5) | 0.6872 (4) | 0.4984 (3) | 0.0242 (11)* | 0.551 (6) |
C12B | 0.0719 (6) | 0.6498 (4) | 0.4382 (3) | 0.0259 (11)* | 0.551 (6) |
C13B | −0.1973 (6) | 0.5896 (5) | 0.4399 (4) | 0.0479 (14)* | 0.551 (6) |
H13B | −0.2896 | 0.5702 | 0.4399 | 0.057* | 0.551 (6) |
C14B | −0.1347 (5) | 0.6545 (4) | 0.4991 (3) | 0.0323 (11)* | 0.551 (6) |
C15B | −0.1255 (6) | 0.5540 (5) | 0.3821 (3) | 0.0374 (12)* | 0.551 (6) |
H15B | −0.1687 | 0.5082 | 0.3435 | 0.045* | 0.551 (6) |
C16B | 0.0088 (5) | 0.7760 (5) | 0.6106 (3) | 0.0343 (13)* | 0.551 (6) |
H16B | 0.058 | 0.8144 | 0.6501 | 0.041* | 0.551 (6) |
C17B | 0.2729 (6) | 0.6438 (5) | 0.3809 (3) | 0.0357 (12)* | 0.551 (6) |
H17B | 0.3647 | 0.6656 | 0.3818 | 0.043* | 0.551 (6) |
C18B | −0.1270 (5) | 0.7503 (5) | 0.6171 (4) | 0.0421 (13)* | 0.551 (6) |
H18B | −0.1697 | 0.7727 | 0.6594 | 0.05* | 0.551 (6) |
C19B | 0.2168 (7) | 0.5783 (5) | 0.3196 (3) | 0.0361 (11)* | 0.551 (6) |
H19B | 0.2683 | 0.5554 | 0.2805 | 0.043* | 0.551 (6) |
C20B | 0.0828 (7) | 0.5499 (5) | 0.3205 (3) | 0.0433 (13)* | 0.551 (6) |
H20B | 0.0399 | 0.5066 | 0.2809 | 0.052* | 0.551 (6) |
C21B | −0.1971 (5) | 0.6912 (5) | 0.5597 (4) | 0.0398 (12)* | 0.551 (6) |
H21B | −0.2897 | 0.6758 | 0.5624 | 0.048* | 0.551 (6) |
O1W | 0.5470 (8) | 0.6539 (8) | 0.2833 (5) | 0.124 (4)* | 0.523 (10) |
O2W | 0 | 0 | 0 | 0.18 (2)* | 0.21 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.02117 (16) | 0.03535 (19) | 0.01631 (16) | −0.00438 (13) | −0.00138 (11) | 0.00062 (13) |
Mn2 | 0.01591 (15) | 0.03624 (19) | 0.01676 (16) | −0.00384 (12) | −0.00053 (11) | 0.00365 (13) |
O1 | 0.0210 (7) | 0.0338 (8) | 0.0194 (7) | 0.0030 (6) | 0.0029 (5) | 0.0027 (6) |
O2 | 0.0254 (7) | 0.0472 (10) | 0.0321 (8) | −0.0084 (7) | −0.0035 (6) | 0.0183 (7) |
O3 | 0.0415 (9) | 0.0621 (12) | 0.0293 (9) | −0.0217 (9) | −0.0150 (7) | 0.0203 (8) |
O4 | 0.0333 (8) | 0.0407 (9) | 0.0228 (8) | −0.0065 (7) | −0.0099 (6) | 0.0059 (7) |
O5 | 0.0206 (7) | 0.0543 (10) | 0.0319 (8) | 0.0090 (7) | −0.0051 (6) | −0.0015 (8) |
O6 | 0.0298 (8) | 0.0604 (12) | 0.0336 (9) | −0.0025 (8) | 0.0054 (7) | 0.0232 (8) |
O7 | 0.0200 (8) | 0.0656 (12) | 0.0518 (11) | 0.0037 (8) | 0.0044 (7) | 0.0240 (10) |
C1 | 0.0219 (9) | 0.0275 (10) | 0.0206 (10) | −0.0032 (8) | −0.0004 (7) | 0.0045 (8) |
C2 | 0.0172 (9) | 0.0293 (10) | 0.0224 (10) | −0.0019 (7) | 0.0007 (7) | 0.0015 (8) |
C3 | 0.0185 (9) | 0.0252 (10) | 0.0207 (9) | 0.0003 (7) | −0.0031 (7) | −0.0003 (8) |
C4 | 0.0232 (9) | 0.0271 (10) | 0.0190 (9) | −0.0001 (8) | −0.0012 (7) | 0.0032 (8) |
C5 | 0.0194 (9) | 0.0293 (10) | 0.0225 (10) | −0.0014 (8) | 0.0004 (7) | 0.0032 (8) |
C6 | 0.0183 (9) | 0.0320 (11) | 0.0248 (10) | −0.0003 (8) | −0.0034 (7) | 0.0059 (8) |
C7 | 0.0232 (10) | 0.0378 (12) | 0.0234 (10) | −0.0026 (9) | −0.0017 (8) | 0.0084 (9) |
C8 | 0.0217 (9) | 0.0261 (10) | 0.0270 (11) | −0.0017 (8) | −0.0070 (8) | −0.0004 (8) |
C9 | 0.0225 (10) | 0.0377 (12) | 0.0222 (10) | −0.0023 (9) | 0.0022 (8) | 0.0029 (9) |
Mn1—O3 | 2.1241 (17) | C5—C6 | 1.388 (3) |
Mn1—O6i | 2.1665 (18) | C5—C9 | 1.491 (3) |
Mn1—O1 | 2.1697 (14) | N1A—C17A | 1.329 (8) |
Mn1—O4ii | 2.1799 (16) | N1A—C12A | 1.365 (8) |
Mn1—N1A | 2.227 (5) | N2A—C16A | 1.343 (8) |
Mn1—N2A | 2.266 (6) | N2A—C11A | 1.378 (9) |
Mn1—N2B | 2.303 (5) | C10A—C20A | 1.369 (9) |
Mn1—N1B | 2.332 (4) | C10A—C15A | 1.406 (9) |
Mn2—O5ii | 2.1209 (15) | C10A—C12A | 1.408 (7) |
Mn2—O1 | 2.1508 (15) | C11A—C12A | 1.410 (8) |
Mn2—O2iii | 2.1696 (16) | C11A—C14A | 1.423 (7) |
Mn2—O1iii | 2.2229 (15) | C13A—C15A | 1.384 (9) |
Mn2—O6iv | 2.3043 (16) | C13A—C14A | 1.430 (9) |
Mn2—O7iv | 2.3695 (17) | C14A—C21A | 1.390 (9) |
O1—Mn2iii | 2.2229 (15) | C16A—C18A | 1.422 (9) |
O2—C7 | 1.253 (3) | C17A—C19A | 1.405 (9) |
O2—Mn2iii | 2.1696 (16) | C18A—C21A | 1.373 (10) |
O3—C7 | 1.259 (3) | C19A—C20A | 1.385 (9) |
O4—C8 | 1.259 (3) | N1B—C17B | 1.342 (6) |
O4—Mn1v | 2.1799 (16) | N1B—C12B | 1.356 (7) |
O5—C8 | 1.253 (3) | N2B—C16B | 1.311 (7) |
O5—Mn2v | 2.1209 (15) | N2B—C11B | 1.358 (7) |
O6—C9 | 1.257 (3) | C10B—C15B | 1.392 (8) |
O6—Mn1vi | 2.1665 (17) | C10B—C20B | 1.407 (7) |
O6—Mn2vii | 2.3043 (16) | C10B—C12B | 1.415 (6) |
O7—C9 | 1.244 (3) | C11B—C14B | 1.408 (6) |
O7—Mn2vii | 2.3695 (17) | C11B—C12B | 1.422 (7) |
C1—C6 | 1.387 (3) | C13B—C15B | 1.386 (7) |
C1—C2 | 1.397 (3) | C13B—C14B | 1.413 (7) |
C1—C7 | 1.504 (3) | C14B—C21B | 1.380 (8) |
C2—C3 | 1.390 (3) | C16B—C18B | 1.404 (7) |
C3—C4 | 1.391 (3) | C17B—C19B | 1.422 (7) |
C3—C8 | 1.504 (3) | C18B—C21B | 1.391 (8) |
C4—C5 | 1.393 (3) | C19B—C20B | 1.382 (7) |
O3—Mn1—O6i | 87.45 (8) | C4—C5—C9 | 119.74 (18) |
O3—Mn1—O1 | 93.36 (6) | C1—C6—C5 | 120.65 (18) |
O6i—Mn1—O1 | 82.52 (6) | O2—C7—O3 | 126.5 (2) |
O3—Mn1—O4ii | 169.92 (7) | O2—C7—C1 | 117.41 (18) |
O6i—Mn1—O4ii | 83.05 (7) | O3—C7—C1 | 116.11 (19) |
O1—Mn1—O4ii | 88.77 (6) | O5—C8—O4 | 124.36 (19) |
O3—Mn1—N1A | 104.44 (15) | O5—C8—C3 | 117.24 (19) |
O6i—Mn1—N1A | 167.89 (15) | O4—C8—C3 | 118.40 (19) |
O1—Mn1—N1A | 94.30 (17) | O7—C9—O6 | 120.2 (2) |
O4ii—Mn1—N1A | 85.21 (14) | O7—C9—C5 | 121.4 (2) |
O3—Mn1—N2A | 90.99 (19) | O6—C9—C5 | 118.45 (19) |
O6i—Mn1—N2A | 108.13 (18) | C17A—N1A—C12A | 117.4 (6) |
O1—Mn1—N2A | 168.68 (18) | C17A—N1A—Mn1 | 126.6 (5) |
O4ii—Mn1—N2A | 88.77 (19) | C12A—N1A—Mn1 | 114.7 (4) |
N1A—Mn1—N2A | 74.5 (2) | C16A—N2A—C11A | 118.9 (6) |
O3—Mn1—N2B | 86.60 (15) | C16A—N2A—Mn1 | 128.4 (5) |
O6i—Mn1—N2B | 102.88 (15) | C11A—N2A—Mn1 | 112.3 (5) |
O1—Mn1—N2B | 174.59 (15) | C20A—C10A—C15A | 123.6 (6) |
O4ii—Mn1—N2B | 92.21 (15) | C20A—C10A—C12A | 115.2 (6) |
N1A—Mn1—N2B | 80.5 (2) | C15A—C10A—C12A | 121.2 (7) |
N2A—Mn1—N2B | 6.7 (2) | N2A—C11A—C12A | 119.3 (5) |
O3—Mn1—N1B | 104.40 (12) | N2A—C11A—C14A | 119.3 (7) |
O6i—Mn1—N1B | 166.24 (12) | C12A—C11A—C14A | 121.4 (6) |
O1—Mn1—N1B | 103.39 (14) | N1A—C12A—C10A | 124.9 (6) |
O4ii—Mn1—N1B | 84.64 (11) | N1A—C12A—C11A | 117.7 (5) |
N1A—Mn1—N1B | 9.13 (16) | C10A—C12A—C11A | 117.4 (6) |
N2A—Mn1—N1B | 65.4 (2) | C15A—C13A—C14A | 117.6 (6) |
N2B—Mn1—N1B | 71.42 (19) | C21A—C14A—C11A | 118.7 (6) |
O5ii—Mn2—O1 | 99.30 (6) | C21A—C14A—C13A | 121.2 (6) |
O5ii—Mn2—O2iii | 87.66 (7) | C11A—C14A—C13A | 120.1 (7) |
O1—Mn2—O2iii | 166.01 (6) | C13A—C15A—C10A | 122.3 (6) |
O5ii—Mn2—O1iii | 141.62 (6) | N2A—C16A—C18A | 125.5 (7) |
O1—Mn2—O1iii | 79.70 (6) | N1A—C17A—C19A | 122.0 (7) |
O2iii—Mn2—O1iii | 87.29 (6) | C21A—C18A—C16A | 114.0 (6) |
O5ii—Mn2—O6iv | 139.59 (6) | C20A—C19A—C17A | 118.7 (7) |
O1—Mn2—O6iv | 93.26 (6) | C10A—C20A—C19A | 121.8 (6) |
O2iii—Mn2—O6iv | 89.11 (7) | C18A—C21A—C14A | 123.6 (6) |
O1iii—Mn2—O6iv | 78.32 (5) | C17B—N1B—C12B | 120.5 (5) |
O5ii—Mn2—O7iv | 85.53 (6) | C17B—N1B—Mn1 | 124.2 (4) |
O1—Mn2—O7iv | 93.99 (7) | C12B—N1B—Mn1 | 113.5 (3) |
O2iii—Mn2—O7iv | 98.66 (7) | C16B—N2B—C11B | 117.9 (5) |
O1iii—Mn2—O7iv | 132.83 (5) | C16B—N2B—Mn1 | 126.0 (4) |
O6iv—Mn2—O7iv | 55.22 (6) | C11B—N2B—Mn1 | 115.4 (4) |
Mn2—O1—Mn1 | 113.60 (6) | C15B—C10B—C20B | 121.9 (5) |
Mn2—O1—Mn2iii | 100.30 (6) | C15B—C10B—C12B | 118.3 (6) |
Mn1—O1—Mn2iii | 97.06 (5) | C20B—C10B—C12B | 119.7 (5) |
C7—O2—Mn2iii | 127.09 (14) | N2B—C11B—C14B | 124.6 (5) |
C7—O3—Mn1 | 128.50 (16) | N2B—C11B—C12B | 117.3 (4) |
C8—O4—Mn1v | 121.85 (14) | C14B—C11B—C12B | 118.1 (5) |
C8—O5—Mn2v | 114.91 (14) | N1B—C12B—C10B | 119.1 (6) |
C9—O6—Mn1vi | 166.07 (17) | N1B—C12B—C11B | 119.2 (4) |
C9—O6—Mn2vii | 93.67 (13) | C10B—C12B—C11B | 121.7 (5) |
Mn1vi—O6—Mn2vii | 94.77 (6) | C15B—C13B—C14B | 120.6 (5) |
C9—O7—Mn2vii | 90.95 (14) | C21B—C14B—C11B | 115.2 (5) |
C6—C1—C2 | 119.50 (19) | C21B—C14B—C13B | 124.8 (5) |
C6—C1—C7 | 119.60 (18) | C11B—C14B—C13B | 120.0 (6) |
C2—C1—C7 | 120.88 (18) | C13B—C15B—C10B | 121.2 (5) |
C3—C2—C1 | 120.01 (18) | N2B—C16B—C18B | 122.6 (6) |
C2—C3—C4 | 120.10 (18) | N1B—C17B—C19B | 123.7 (6) |
C2—C3—C8 | 120.81 (18) | C21B—C18B—C16B | 118.1 (5) |
C4—C3—C8 | 119.08 (18) | C20B—C19B—C17B | 115.9 (5) |
C3—C4—C5 | 119.88 (18) | C19B—C20B—C10B | 121.0 (5) |
C6—C5—C4 | 119.76 (18) | C14B—C21B—C18B | 121.3 (5) |
C6—C5—C9 | 120.46 (18) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+3/2; (ii) x−1/2, −y+3/2, z−1/2; (iii) −x+1, −y+2, −z+1; (iv) x+1/2, −y+3/2, z−1/2; (v) x+1/2, −y+3/2, z+1/2; (vi) −x+1/2, y−1/2, −z+3/2; (vii) x−1/2, −y+3/2, z+1/2. |