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In recent years, crystalline polyoxotitanium clusters (PTCs) have attracted increasing attention as a new kind of promising crystalline material. In this work, a PTC stabilized by phenylphosphonate ligands, i.e. hexa-μ-isopropanolato-hexaisopropanolatodi-μ3-oxido-hexa-μ3-phenylphosphonato-heptatitanium tetrahydrate, [Ti7(μ3-O)2(O3P-Phen)6(OiPr)12]·4H2O [PTC-54; H2O3P-Phen is phenylphosphonic acid, C6H5PO(OH)2, and HOiPr is isopropanol, C3H7OH], was obtained successfully through a facile one-step solvothermal reaction. The dumbbell-like core structure of PTC-54 can be described as two trinuclear {Ti3(μ3-O)} building units combined together by six phenylphosphonate ligands and one additional Ti atom, giving rise to a Ti7 cluster. Adjacent molecules of PTC-54 are further connected through π–π interactions between the phenyl groups to form a supramolecular one-dimensional chain.
Supporting information
CCDC reference: 1843756
Data collection: Please provide references for software used for data collection, cell
refinement, data reduction, structure solution and molecular graphics; program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015).
Hexa-µ-isopropanolato-hexaisopropanolatodi-µ
3-oxido-hexa-µ
3-\
phenylphosphonato-heptatitanium tetrahydrate
top
Crystal data top
[Ti7O2(C6H5O3P)6(C3H7O)12]·4H2O | F(000) = 4176 |
Mr = 2010.73 | Dx = 1.319 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 23.073 (4) Å | Cell parameters from 13036 reflections |
b = 12.9877 (19) Å | θ = 2.0–27.5° |
c = 34.994 (5) Å | µ = 0.69 mm−1 |
β = 105.158 (3)° | T = 293 K |
V = 10122 (3) Å3 | Strip, colorless |
Z = 4 | 0.5 × 0.3 × 0.25 mm |
Data collection top
Saturn724+ (2x2 bin mode) diffractometer | 9545 reflections with I > 2σ(I) |
CCD_Profile_fitting scans | Rint = 0.026 |
Absorption correction: multi-scan (REFERENCE?) | θmax = 27.5°, θmin = 2.0° |
Tmin = 0.838, Tmax = 1.000 | h = −24→29 |
37753 measured reflections | k = −16→16 |
11330 independent reflections | l = −45→45 |
Refinement top
Refinement on F2 | 452 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.067 | H-atom parameters constrained |
wR(F2) = 0.235 | w = 1/[σ2(Fo2) + (0.1774P)2 + 10.8217P] where P = (Fo2 + 2Fc2)/3 |
S = 0.94 | (Δ/σ)max = 0.004 |
11330 reflections | Δρmax = 1.10 e Å−3 |
541 parameters | Δρmin = −0.95 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ti1 | 0.2500 | 0.7500 | 0.0000 | 0.03929 (19) | |
Ti2 | 0.35945 (3) | 0.66303 (5) | 0.13197 (2) | 0.05656 (19) | |
Ti3 | 0.22514 (3) | 0.60260 (5) | 0.11959 (2) | 0.0584 (2) | |
Ti4 | 0.26528 (3) | 0.83069 (5) | 0.13597 (2) | 0.05657 (19) | |
P5 | 0.34800 (4) | 0.85942 (6) | 0.07900 (2) | 0.0464 (2) | |
P6 | 0.16054 (4) | 0.77619 (6) | 0.06246 (2) | 0.0472 (2) | |
P7 | 0.29323 (4) | 0.53886 (6) | 0.05722 (2) | 0.0468 (2) | |
O1 | 0.27758 (10) | 0.70842 (16) | 0.10653 (6) | 0.0467 (5) | |
O2 | 0.27426 (10) | 0.62259 (16) | 0.02650 (6) | 0.0485 (5) | |
O3 | 0.19022 (11) | 0.85473 (17) | 0.09434 (7) | 0.0542 (5) | |
O4 | 0.35208 (11) | 0.56465 (18) | 0.08798 (7) | 0.0548 (5) | |
O5 | 0.30948 (10) | 0.82360 (17) | 0.03929 (6) | 0.0490 (5) | |
O6 | 0.15798 (11) | 0.66969 (18) | 0.08110 (8) | 0.0558 (5) | |
O7 | 0.24355 (11) | 0.51557 (17) | 0.07827 (7) | 0.0562 (6) | |
O8 | 0.31102 (11) | 0.90870 (17) | 0.10521 (7) | 0.0535 (5) | |
O9 | 0.22152 (14) | 0.7192 (2) | 0.15811 (8) | 0.0704 (7) | |
O10 | 0.38747 (10) | 0.77219 (18) | 0.10156 (7) | 0.0538 (5) | |
O11 | 0.19060 (10) | 0.77063 (17) | 0.02888 (6) | 0.0498 (5) | |
O12 | 0.25663 (15) | 0.9367 (2) | 0.16596 (8) | 0.0774 (8) | |
O13 | 0.30742 (14) | 0.5668 (2) | 0.15488 (7) | 0.0689 (7) | |
O14 | 0.34474 (13) | 0.7739 (2) | 0.16925 (7) | 0.0681 (7) | |
C0AA | 0.39677 (16) | 0.9562 (3) | 0.06801 (13) | 0.0635 (9) | |
O16 | 0.43223 (14) | 0.6211 (2) | 0.15860 (8) | 0.0738 (7) | |
C17 | 0.30551 (16) | 0.4268 (3) | 0.03063 (13) | 0.0603 (8) | |
O18 | 0.18039 (15) | 0.5103 (2) | 0.13599 (9) | 0.0781 (8) | |
C1AA | 0.08539 (15) | 0.8191 (3) | 0.04023 (13) | 0.0604 (8) | |
C2AA | 0.0505 (2) | 0.8644 (4) | 0.06224 (18) | 0.0840 (11) | |
H2AA | 0.0671 | 0.8753 | 0.0891 | 0.101* | |
C21 | 0.2944 (2) | 0.4291 (3) | −0.00986 (15) | 0.0751 (10) | |
H21 | 0.2811 | 0.4893 | −0.0238 | 0.090* | |
C23 | 0.3269 (2) | 0.3351 (3) | 0.05041 (17) | 0.0795 (11) | |
H23 | 0.3358 | 0.3327 | 0.0779 | 0.095* | |
C24 | 0.3035 (2) | 0.3384 (4) | −0.03022 (19) | 0.0924 (13) | |
H24 | 0.2958 | 0.3386 | −0.0577 | 0.111* | |
C27 | 0.3349 (2) | 0.2487 (3) | 0.02979 (19) | 0.0870 (12) | |
H27 | 0.3485 | 0.1881 | 0.0433 | 0.104* | |
C29 | 0.0603 (2) | 0.8049 (4) | 0.00066 (16) | 0.0815 (11) | |
H29 | 0.0826 | 0.7765 | −0.0153 | 0.098* | |
C31 | 0.4404 (2) | 1.0414 (4) | 0.0211 (2) | 0.0929 (12) | |
H31 | 0.4437 | 1.0490 | −0.0046 | 0.111* | |
C33 | 0.4012 (2) | 0.9691 (3) | 0.02969 (16) | 0.0779 (10) | |
H33 | 0.3778 | 0.9290 | 0.0094 | 0.094* | |
C36 | 0.4300 (2) | 1.0176 (4) | 0.09704 (19) | 0.0992 (14) | |
H36 | 0.4274 | 1.0116 | 0.1230 | 0.119* | |
C3AA | −0.0075 (2) | 0.8935 (4) | 0.0458 (2) | 0.0957 (13) | |
H3AA | −0.0297 | 0.9239 | 0.0615 | 0.115* | |
C2 | 0.3235 (2) | 0.2514 (4) | −0.00936 (19) | 0.0892 (12) | |
H2 | 0.3293 | 0.1922 | −0.0229 | 0.107* | |
C3 | −0.0323 (2) | 0.8788 (4) | 0.0077 (2) | 0.0931 (13) | |
H3 | −0.0718 | 0.8989 | −0.0033 | 0.112* | |
C6AA | −0.0001 (2) | 0.8340 (4) | −0.0156 (2) | 0.1008 (15) | |
H6AA | −0.0181 | 0.8227 | −0.0423 | 0.121* | |
C6 | 0.3852 (3) | 0.8183 (6) | 0.20319 (16) | 0.126 (2) | |
H6 | 0.3588 | 0.8746 | 0.2066 | 0.151* | |
C7AA | 0.1851 (3) | 0.7216 (6) | 0.18529 (16) | 0.118 (2) | |
H7AA | 0.1769 | 0.6492 | 0.1896 | 0.142* | |
C8 | 0.2512 (4) | 1.0375 (5) | 0.1791 (3) | 0.165 (3) | |
H8 | 0.2631 | 1.0391 | 0.2081 | 0.198* | |
C9 | 0.4695 (3) | 1.0923 (5) | 0.0866 (2) | 0.1142 (17) | |
H9 | 0.4923 | 1.1353 | 0.1061 | 0.137* | |
C11 | 0.3254 (4) | 0.4837 (5) | 0.18168 (17) | 0.132 (2) | |
H11 | 0.2843 | 0.4651 | 0.1819 | 0.159* | |
C12 | 0.3364 (5) | 0.3873 (5) | 0.1626 (2) | 0.160 (3) | |
H12A | 0.3096 | 0.3832 | 0.1365 | 0.240* | |
H12B | 0.3297 | 0.3297 | 0.1781 | 0.240* | |
H12C | 0.3772 | 0.3861 | 0.1606 | 0.240* | |
C4AA | 0.1246 (4) | 0.7680 (8) | 0.1672 (2) | 0.158 (3) | |
H4AA | 0.1272 | 0.8416 | 0.1697 | 0.238* | |
H4AB | 0.0963 | 0.7425 | 0.1807 | 0.238* | |
H4AC | 0.1116 | 0.7496 | 0.1398 | 0.238* | |
C5AA | 0.1373 (5) | 0.4388 (8) | 0.1326 (3) | 0.181 (3) | |
H5AA | 0.1065 | 0.4886 | 0.1196 | 0.217* | |
C15 | 0.4324 (4) | 0.8840 (7) | 0.1946 (2) | 0.171 (4) | |
H15A | 0.4491 | 0.8506 | 0.1754 | 0.256* | |
H15B | 0.4634 | 0.8954 | 0.2185 | 0.256* | |
H15C | 0.4153 | 0.9489 | 0.1842 | 0.256* | |
C16 | 0.2206 (5) | 0.7597 (9) | 0.22503 (19) | 0.192 (4) | |
H16A | 0.2101 | 0.7203 | 0.2455 | 0.288* | |
H16B | 0.2115 | 0.8310 | 0.2279 | 0.288* | |
H16C | 0.2627 | 0.7521 | 0.2272 | 0.288* | |
C18 | 0.4911 (3) | 0.5926 (7) | 0.1632 (3) | 0.143 (2) | |
C19 | 0.1238 (6) | 0.3754 (9) | 0.0980 (3) | 0.225 (5) | |
H19A | 0.1247 | 0.4165 | 0.0753 | 0.337* | |
H19B | 0.0846 | 0.3458 | 0.0942 | 0.337* | |
H19C | 0.1531 | 0.3215 | 0.1011 | 0.337* | |
C1 | 0.4736 (2) | 1.1006 (4) | 0.0506 (2) | 0.1031 (14) | |
H1 | 0.5001 | 1.1484 | 0.0448 | 0.124* | |
C4 | 0.1867 (4) | 1.0712 (8) | 0.1642 (4) | 0.220 (5) | |
H4A | 0.1770 | 1.0800 | 0.1360 | 0.329* | |
H4B | 0.1811 | 1.1352 | 0.1765 | 0.329* | |
H4C | 0.1610 | 1.0198 | 0.1707 | 0.329* | |
C7 | 0.5222 (5) | 0.6415 (10) | 0.1350 (4) | 0.217 (4) | |
H7A | 0.5121 | 0.7133 | 0.1322 | 0.326* | |
H7B | 0.5095 | 0.6083 | 0.1097 | 0.326* | |
H7C | 0.5649 | 0.6341 | 0.1452 | 0.326* | |
C8AA | 0.1101 (6) | 0.4296 (10) | 0.1661 (3) | 0.229 (5) | |
H8AA | 0.1377 | 0.3957 | 0.1878 | 0.344* | |
H8AB | 0.0737 | 0.3901 | 0.1581 | 0.344* | |
H8AC | 0.1010 | 0.4969 | 0.1743 | 0.344* | |
C10 | 0.2881 (5) | 1.1087 (7) | 0.1640 (4) | 0.221 (5) | |
H10A | 0.3234 | 1.0740 | 0.1612 | 0.332* | |
H10B | 0.2995 | 1.1652 | 0.1821 | 0.332* | |
H10C | 0.2657 | 1.1343 | 0.1387 | 0.332* | |
C14 | 0.5126 (5) | 0.5001 (9) | 0.1861 (4) | 0.226 (5) | |
H14A | 0.4890 | 0.4879 | 0.2045 | 0.339* | |
H14B | 0.5539 | 0.5091 | 0.2003 | 0.339* | |
H14C | 0.5090 | 0.4423 | 0.1685 | 0.339* | |
C5 | 0.3833 (6) | 0.7614 (10) | 0.2391 (2) | 0.231 (4) | |
H5A | 0.3831 | 0.8092 | 0.2600 | 0.347* | |
H5B | 0.4179 | 0.7176 | 0.2470 | 0.347* | |
H5C | 0.3475 | 0.7202 | 0.2338 | 0.347* | |
C9AA | 0.3426 (6) | 0.5151 (8) | 0.2230 (2) | 0.214 (4) | |
H9AA | 0.3683 | 0.4637 | 0.2384 | 0.320* | |
H9AB | 0.3073 | 0.5228 | 0.2323 | 0.320* | |
H9AC | 0.3636 | 0.5796 | 0.2254 | 0.320* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ti1 | 0.0340 (4) | 0.0370 (3) | 0.0469 (4) | −0.0026 (3) | 0.0107 (3) | 0.0005 (3) |
Ti2 | 0.0549 (4) | 0.0545 (4) | 0.0536 (3) | 0.0027 (3) | 0.0021 (3) | 0.0064 (2) |
Ti3 | 0.0659 (4) | 0.0510 (3) | 0.0640 (4) | −0.0034 (3) | 0.0274 (3) | 0.0113 (3) |
Ti4 | 0.0636 (4) | 0.0543 (4) | 0.0533 (3) | −0.0023 (3) | 0.0181 (3) | −0.0073 (2) |
P5 | 0.0395 (4) | 0.0415 (4) | 0.0550 (4) | −0.0068 (3) | 0.0065 (3) | −0.0027 (3) |
P6 | 0.0413 (4) | 0.0429 (4) | 0.0619 (5) | −0.0026 (3) | 0.0214 (4) | −0.0007 (3) |
P7 | 0.0443 (4) | 0.0352 (4) | 0.0602 (4) | 0.0004 (3) | 0.0123 (3) | 0.0041 (3) |
O1 | 0.0487 (12) | 0.0429 (10) | 0.0493 (10) | −0.0010 (9) | 0.0143 (9) | 0.0024 (8) |
O2 | 0.0499 (12) | 0.0399 (10) | 0.0551 (11) | 0.0011 (9) | 0.0126 (10) | 0.0041 (8) |
O3 | 0.0537 (13) | 0.0487 (12) | 0.0632 (13) | −0.0002 (10) | 0.0208 (11) | −0.0052 (10) |
O4 | 0.0493 (13) | 0.0467 (11) | 0.0639 (13) | 0.0022 (9) | 0.0067 (10) | 0.0054 (10) |
O5 | 0.0425 (12) | 0.0494 (11) | 0.0527 (11) | −0.0082 (9) | 0.0081 (9) | −0.0010 (9) |
O6 | 0.0530 (13) | 0.0486 (12) | 0.0714 (14) | −0.0052 (10) | 0.0260 (11) | 0.0048 (10) |
O7 | 0.0594 (14) | 0.0417 (11) | 0.0700 (14) | −0.0048 (10) | 0.0212 (12) | 0.0079 (10) |
O8 | 0.0538 (13) | 0.0460 (11) | 0.0593 (12) | −0.0051 (9) | 0.0126 (10) | −0.0058 (9) |
O9 | 0.088 (2) | 0.0733 (17) | 0.0607 (14) | −0.0024 (14) | 0.0381 (14) | 0.0032 (12) |
O10 | 0.0441 (12) | 0.0497 (12) | 0.0625 (12) | −0.0021 (9) | 0.0048 (10) | 0.0012 (10) |
O11 | 0.0410 (11) | 0.0548 (12) | 0.0565 (11) | 0.0008 (9) | 0.0176 (9) | 0.0006 (9) |
O12 | 0.095 (2) | 0.0710 (17) | 0.0692 (15) | 0.0002 (16) | 0.0274 (15) | −0.0215 (13) |
O13 | 0.0833 (19) | 0.0627 (15) | 0.0597 (13) | 0.0060 (13) | 0.0171 (13) | 0.0194 (12) |
O14 | 0.0727 (18) | 0.0764 (17) | 0.0493 (12) | 0.0017 (14) | 0.0054 (12) | −0.0033 (11) |
C0AA | 0.0445 (17) | 0.0461 (16) | 0.099 (2) | −0.0080 (13) | 0.0162 (17) | 0.0051 (16) |
O16 | 0.0657 (15) | 0.0723 (16) | 0.0707 (16) | 0.0088 (13) | −0.0048 (13) | 0.0113 (13) |
C17 | 0.0456 (17) | 0.0430 (15) | 0.094 (2) | −0.0004 (13) | 0.0216 (16) | −0.0038 (15) |
O18 | 0.087 (2) | 0.0673 (17) | 0.0915 (19) | −0.0086 (15) | 0.0437 (17) | 0.0193 (15) |
C1AA | 0.0401 (16) | 0.0490 (16) | 0.095 (2) | −0.0044 (13) | 0.0235 (16) | 0.0014 (16) |
C2AA | 0.055 (2) | 0.086 (2) | 0.118 (3) | 0.0061 (19) | 0.036 (2) | −0.006 (2) |
C21 | 0.069 (2) | 0.0560 (19) | 0.101 (2) | 0.0030 (17) | 0.022 (2) | −0.0195 (19) |
C23 | 0.066 (2) | 0.0491 (18) | 0.122 (3) | 0.0086 (16) | 0.022 (2) | −0.0010 (19) |
C24 | 0.082 (3) | 0.080 (3) | 0.115 (3) | 0.003 (2) | 0.027 (2) | −0.031 (2) |
C27 | 0.070 (2) | 0.0518 (19) | 0.138 (3) | 0.0101 (17) | 0.024 (2) | −0.009 (2) |
C29 | 0.054 (2) | 0.076 (2) | 0.110 (3) | 0.0106 (18) | 0.014 (2) | 0.002 (2) |
C31 | 0.083 (3) | 0.073 (2) | 0.136 (3) | −0.002 (2) | 0.052 (2) | 0.019 (2) |
C33 | 0.074 (2) | 0.0570 (19) | 0.117 (3) | −0.0059 (17) | 0.049 (2) | 0.0032 (19) |
C36 | 0.079 (3) | 0.082 (3) | 0.126 (3) | −0.037 (2) | 0.007 (3) | 0.001 (2) |
C3AA | 0.059 (2) | 0.097 (3) | 0.138 (3) | 0.013 (2) | 0.038 (2) | 0.003 (3) |
C2 | 0.071 (2) | 0.060 (2) | 0.139 (3) | 0.0044 (18) | 0.032 (2) | −0.030 (2) |
C3 | 0.048 (2) | 0.082 (3) | 0.146 (3) | 0.0045 (19) | 0.020 (2) | 0.009 (3) |
C6AA | 0.070 (3) | 0.094 (3) | 0.125 (3) | 0.000 (2) | 0.002 (3) | 0.006 (3) |
C6 | 0.136 (5) | 0.148 (5) | 0.073 (3) | −0.011 (4) | −0.010 (3) | −0.034 (3) |
C7AA | 0.140 (5) | 0.149 (5) | 0.093 (3) | 0.005 (4) | 0.079 (4) | 0.011 (3) |
C8 | 0.168 (7) | 0.082 (4) | 0.269 (9) | 0.001 (4) | 0.096 (7) | −0.069 (5) |
C9 | 0.089 (3) | 0.085 (3) | 0.152 (4) | −0.036 (2) | 0.001 (3) | 0.005 (3) |
C11 | 0.187 (7) | 0.103 (4) | 0.108 (3) | 0.029 (4) | 0.040 (4) | 0.066 (3) |
C12 | 0.235 (9) | 0.088 (4) | 0.147 (6) | 0.038 (5) | 0.029 (6) | 0.048 (4) |
C4AA | 0.145 (6) | 0.221 (8) | 0.143 (5) | 0.038 (6) | 0.097 (5) | 0.025 (6) |
C5AA | 0.211 (7) | 0.187 (6) | 0.174 (6) | −0.117 (5) | 0.105 (5) | −0.018 (5) |
C15 | 0.187 (8) | 0.176 (7) | 0.110 (5) | −0.072 (6) | −0.031 (5) | −0.015 (5) |
C16 | 0.238 (8) | 0.263 (9) | 0.094 (4) | 0.025 (7) | 0.077 (5) | −0.005 (5) |
C18 | 0.081 (3) | 0.167 (5) | 0.175 (5) | 0.040 (3) | 0.025 (3) | 0.041 (4) |
C19 | 0.295 (10) | 0.206 (9) | 0.204 (8) | −0.161 (8) | 0.120 (8) | −0.065 (7) |
C1 | 0.072 (3) | 0.081 (3) | 0.160 (4) | −0.019 (2) | 0.037 (3) | 0.015 (3) |
C4 | 0.177 (8) | 0.120 (6) | 0.375 (12) | 0.030 (6) | 0.095 (9) | −0.038 (8) |
C7 | 0.130 (7) | 0.255 (10) | 0.291 (10) | 0.037 (7) | 0.097 (7) | 0.071 (9) |
C8AA | 0.284 (10) | 0.239 (9) | 0.219 (8) | −0.142 (8) | 0.163 (8) | −0.034 (7) |
C10 | 0.207 (9) | 0.086 (5) | 0.372 (12) | −0.039 (5) | 0.077 (9) | −0.031 (7) |
C14 | 0.141 (7) | 0.222 (9) | 0.316 (11) | 0.084 (7) | 0.059 (8) | 0.100 (8) |
C5 | 0.291 (8) | 0.262 (8) | 0.108 (5) | −0.056 (7) | −0.009 (6) | 0.005 (6) |
C9AA | 0.312 (9) | 0.194 (7) | 0.109 (3) | 0.025 (7) | 0.010 (6) | 0.053 (5) |
Geometric parameters (Å, º) top
Ti1—O2 | 1.908 (2) | P7—C17 | 1.790 (4) |
Ti1—O2i | 1.908 (2) | O9—C7AA | 1.424 (5) |
Ti1—O11 | 1.922 (2) | O12—C8 | 1.404 (6) |
Ti1—O11i | 1.922 (2) | O13—C11 | 1.419 (5) |
Ti1—O5i | 1.924 (2) | O14—C6 | 1.427 (6) |
Ti1—O5 | 1.924 (2) | C0AA—C36 | 1.360 (6) |
Ti2—O16 | 1.780 (3) | C0AA—C33 | 1.382 (6) |
Ti2—O1 | 1.957 (2) | O16—C18 | 1.375 (7) |
Ti2—O4 | 1.973 (2) | C17—C21 | 1.373 (6) |
Ti2—O10 | 1.980 (2) | C17—C23 | 1.401 (6) |
Ti2—O14 | 2.030 (3) | O18—C5AA | 1.343 (8) |
Ti2—O13 | 2.037 (3) | C1AA—C29 | 1.367 (6) |
Ti2—Ti4 | 3.1050 (10) | C1AA—C2AA | 1.382 (6) |
Ti2—Ti3 | 3.1153 (11) | C2AA—C3AA | 1.366 (7) |
Ti3—O18 | 1.773 (3) | C21—C24 | 1.420 (6) |
Ti3—O1 | 1.962 (2) | C23—C27 | 1.372 (6) |
Ti3—O7 | 1.967 (3) | C24—C2 | 1.359 (8) |
Ti3—O6 | 1.971 (3) | C27—C2 | 1.326 (8) |
Ti3—O13 | 2.030 (3) | C29—C6AA | 1.412 (7) |
Ti3—O9 | 2.043 (3) | C31—C1 | 1.353 (8) |
Ti3—Ti4 | 3.1121 (10) | C31—C33 | 1.389 (6) |
Ti4—O12 | 1.773 (3) | C36—C9 | 1.441 (8) |
Ti4—O1 | 1.954 (2) | C3AA—C3 | 1.319 (8) |
Ti4—O8 | 1.973 (2) | C3—C6AA | 1.369 (8) |
Ti4—O3 | 1.975 (3) | C6—C5 | 1.470 (8) |
Ti4—O14 | 2.036 (3) | C6—C15 | 1.474 (8) |
Ti4—O9 | 2.032 (3) | C7AA—C16 | 1.501 (7) |
P5—O5 | 1.514 (2) | C7AA—C4AA | 1.500 (7) |
P5—O10 | 1.536 (2) | C8—C10 | 1.447 (13) |
P5—O8 | 1.546 (2) | C8—C4 | 1.507 (8) |
P5—C0AA | 1.795 (4) | C9—C1 | 1.294 (9) |
P6—O11 | 1.514 (2) | C11—C9AA | 1.453 (7) |
P6—O3 | 1.534 (2) | C11—C12 | 1.473 (7) |
P6—O6 | 1.537 (2) | C5AA—C19 | 1.431 (11) |
P6—C1AA | 1.794 (4) | C5AA—C8AA | 1.472 (7) |
P7—O2 | 1.511 (2) | C18—C14 | 1.458 (8) |
P7—O4 | 1.533 (2) | C18—C7 | 1.505 (8) |
P7—O7 | 1.546 (3) | | |
| | | |
O2—Ti1—O2i | 180.0 | O12—Ti4—Ti3 | 140.69 (11) |
O2—Ti1—O11 | 91.39 (10) | O1—Ti4—Ti3 | 37.47 (6) |
O2i—Ti1—O11 | 88.61 (10) | O8—Ti4—Ti3 | 124.34 (7) |
O2—Ti1—O11i | 88.61 (10) | O3—Ti4—Ti3 | 81.56 (7) |
O2i—Ti1—O11i | 91.39 (10) | O14—Ti4—Ti3 | 86.59 (9) |
O11—Ti1—O11i | 180.0 | O9—Ti4—Ti3 | 40.35 (8) |
O2—Ti1—O5i | 88.87 (10) | Ti2—Ti4—Ti3 | 60.14 (2) |
O2i—Ti1—O5i | 91.14 (10) | O5—P5—O10 | 111.83 (13) |
O11—Ti1—O5i | 88.37 (10) | O5—P5—O8 | 112.91 (13) |
O11i—Ti1—O5i | 91.63 (10) | O10—P5—O8 | 110.21 (14) |
O2—Ti1—O5 | 91.13 (10) | O5—P5—C0AA | 105.63 (17) |
O2i—Ti1—O5 | 88.87 (10) | O10—P5—C0AA | 107.82 (16) |
O11—Ti1—O5 | 91.63 (10) | O8—P5—C0AA | 108.14 (16) |
O11i—Ti1—O5 | 88.38 (10) | O11—P6—O3 | 112.83 (13) |
O5i—Ti1—O5 | 180.00 (11) | O11—P6—O6 | 111.26 (13) |
O16—Ti2—O1 | 175.56 (13) | O3—P6—O6 | 110.43 (14) |
O16—Ti2—O4 | 95.01 (12) | O11—P6—C1AA | 105.39 (16) |
O1—Ti2—O4 | 87.95 (9) | O3—P6—C1AA | 107.80 (16) |
O16—Ti2—O10 | 96.00 (13) | O6—P6—C1AA | 108.88 (15) |
O1—Ti2—O10 | 87.24 (9) | O2—P7—O4 | 112.39 (13) |
O4—Ti2—O10 | 91.03 (10) | O2—P7—O7 | 111.52 (13) |
O16—Ti2—O14 | 100.02 (13) | O4—P7—O7 | 109.84 (14) |
O1—Ti2—O14 | 76.99 (10) | O2—P7—C17 | 105.73 (16) |
O4—Ti2—O14 | 164.94 (11) | O4—P7—C17 | 108.13 (16) |
O10—Ti2—O14 | 88.32 (11) | O7—P7—C17 | 109.05 (15) |
O16—Ti2—O13 | 100.29 (13) | Ti2—O1—Ti4 | 105.13 (10) |
O1—Ti2—O13 | 76.45 (10) | Ti2—O1—Ti3 | 105.30 (10) |
O4—Ti2—O13 | 88.30 (11) | Ti4—O1—Ti3 | 105.26 (10) |
O10—Ti2—O13 | 163.69 (11) | P7—O2—Ti1 | 164.46 (15) |
O14—Ti2—O13 | 88.13 (12) | P6—O3—Ti4 | 124.74 (14) |
O16—Ti2—Ti4 | 140.06 (10) | P7—O4—Ti2 | 124.68 (15) |
O1—Ti2—Ti4 | 37.40 (6) | P5—O5—Ti1 | 161.22 (15) |
O4—Ti2—Ti4 | 124.80 (7) | P6—O6—Ti3 | 125.27 (15) |
O10—Ti2—Ti4 | 81.54 (7) | P7—O7—Ti3 | 124.56 (14) |
O14—Ti2—Ti4 | 40.28 (8) | P5—O8—Ti4 | 124.63 (14) |
O13—Ti2—Ti4 | 85.48 (9) | C7AA—O9—Ti4 | 132.6 (4) |
O16—Ti2—Ti3 | 139.81 (11) | C7AA—O9—Ti3 | 126.2 (4) |
O1—Ti2—Ti3 | 37.42 (6) | Ti4—O9—Ti3 | 99.58 (11) |
O4—Ti2—Ti3 | 81.30 (7) | P5—O10—Ti2 | 124.83 (15) |
O10—Ti2—Ti3 | 123.95 (7) | P6—O11—Ti1 | 161.56 (15) |
O14—Ti2—Ti3 | 86.60 (9) | C8—O12—Ti4 | 162.0 (5) |
O13—Ti2—Ti3 | 39.91 (8) | C11—O13—Ti3 | 129.9 (4) |
Ti4—Ti2—Ti3 | 60.04 (2) | C11—O13—Ti2 | 128.8 (4) |
O18—Ti3—O1 | 174.74 (13) | Ti3—O13—Ti2 | 100.01 (10) |
O18—Ti3—O7 | 96.05 (13) | C6—O14—Ti2 | 129.7 (4) |
O1—Ti3—O7 | 88.08 (9) | C6—O14—Ti4 | 128.7 (4) |
O18—Ti3—O6 | 95.74 (13) | Ti2—O14—Ti4 | 99.57 (11) |
O1—Ti3—O6 | 87.34 (9) | C36—C0AA—C33 | 118.9 (4) |
O7—Ti3—O6 | 91.95 (11) | C36—C0AA—P5 | 120.9 (4) |
O18—Ti3—O13 | 100.34 (13) | C33—C0AA—P5 | 120.2 (3) |
O1—Ti3—O13 | 76.49 (10) | C18—O16—Ti2 | 155.7 (4) |
O7—Ti3—O13 | 88.18 (11) | C21—C17—C23 | 118.3 (4) |
O6—Ti3—O13 | 163.83 (11) | C21—C17—P7 | 120.5 (3) |
O18—Ti3—O9 | 99.18 (13) | C23—C17—P7 | 121.2 (4) |
O1—Ti3—O9 | 76.63 (10) | C5AA—O18—Ti3 | 156.9 (5) |
O7—Ti3—O9 | 164.71 (11) | C29—C1AA—C2AA | 117.9 (4) |
O6—Ti3—O9 | 87.87 (11) | C29—C1AA—P6 | 120.2 (3) |
O13—Ti3—O9 | 87.78 (12) | C2AA—C1AA—P6 | 121.9 (4) |
O18—Ti3—Ti4 | 138.99 (11) | C3AA—C2AA—C1AA | 122.2 (5) |
O1—Ti3—Ti4 | 37.27 (6) | C17—C21—C24 | 119.2 (5) |
O7—Ti3—Ti4 | 124.84 (7) | C27—C23—C17 | 120.9 (5) |
O6—Ti3—Ti4 | 81.25 (7) | C2—C24—C21 | 119.6 (5) |
O13—Ti3—Ti4 | 85.41 (8) | C2—C27—C23 | 120.3 (5) |
O9—Ti3—Ti4 | 40.07 (8) | C1AA—C29—C6AA | 119.0 (5) |
O18—Ti3—Ti2 | 140.15 (11) | C1—C31—C33 | 119.4 (6) |
O1—Ti3—Ti2 | 37.29 (6) | C31—C33—C0AA | 120.6 (5) |
O7—Ti3—Ti2 | 81.31 (8) | C0AA—C36—C9 | 118.4 (6) |
O6—Ti3—Ti2 | 124.02 (7) | C3—C3AA—C2AA | 120.1 (5) |
O13—Ti3—Ti2 | 40.08 (8) | C27—C2—C24 | 121.6 (4) |
O9—Ti3—Ti2 | 86.12 (9) | C3AA—C3—C6AA | 120.4 (5) |
Ti4—Ti3—Ti2 | 59.82 (2) | C3—C6AA—C29 | 120.3 (6) |
O12—Ti4—O1 | 175.76 (13) | O14—C6—C5 | 110.4 (7) |
O12—Ti4—O8 | 94.78 (13) | O14—C6—C15 | 114.9 (5) |
O1—Ti4—O8 | 87.57 (9) | C5—C6—C15 | 131.0 (7) |
O12—Ti4—O3 | 95.80 (13) | O9—C7AA—C16 | 110.6 (6) |
O1—Ti4—O3 | 87.69 (9) | O9—C7AA—C4AA | 112.0 (5) |
O8—Ti4—O3 | 90.42 (10) | C16—C7AA—C4AA | 118.6 (7) |
O12—Ti4—O14 | 99.60 (13) | O12—C8—C10 | 111.5 (7) |
O1—Ti4—O14 | 76.93 (10) | O12—C8—C4 | 108.8 (7) |
O8—Ti4—O14 | 88.17 (11) | C10—C8—C4 | 108.1 (10) |
O3—Ti4—O14 | 164.60 (10) | C1—C9—C36 | 121.1 (6) |
O12—Ti4—O9 | 100.58 (14) | O13—C11—C9AA | 113.6 (6) |
O1—Ti4—O9 | 77.10 (10) | O13—C11—C12 | 113.7 (5) |
O8—Ti4—O9 | 164.64 (10) | C9AA—C11—C12 | 131.0 (7) |
O3—Ti4—O9 | 88.08 (11) | O18—C5AA—C19 | 117.6 (7) |
O14—Ti4—O9 | 89.23 (13) | O18—C5AA—C8AA | 116.5 (7) |
O12—Ti4—Ti2 | 139.41 (11) | C19—C5AA—C8AA | 125.8 (8) |
O1—Ti4—Ti2 | 37.47 (6) | O16—C18—C14 | 118.1 (7) |
O8—Ti4—Ti2 | 81.67 (7) | O16—C18—C7 | 115.8 (6) |
O3—Ti4—Ti2 | 124.51 (7) | C14—C18—C7 | 123.7 (8) |
O14—Ti4—Ti2 | 40.15 (8) | C9—C1—C31 | 121.6 (5) |
O9—Ti4—Ti2 | 86.60 (9) | | |
Symmetry code: (i) −x+1/2, −y+3/2, −z. |
Crystal data and structure refinement summary for PTC-54 topCCDC No | 1843756 |
Formula | C72H122O36P6Ti7 |
Mr | 2084.63 |
Crystal system | monoclinic |
Space group | C2/c |
a, b, c(Å) | 23.073 (4), 12.9877 (19), 34.994 (5) |
α, β, γ (°) | 90, 105.158 (3), 90 |
V (Å3) | 10122 (3) |
Z | 4 |
Radiation type | Mo Kα |
T (K) | 293 (2) |
ρc (Mg m-3) | 1.321 |
µ (mm-1) | 0.688 |
Crystal size (mm) | 0.50 × 0.30 × 0.25 |
Absorption correction | Multi-scan (reference?) |
Tmin, Tmax | 0.8381, 1.0000 |
Data/restraints/parameters | 11330/452/541 |
Reflections collected | 37731 |
Unique reflections | 11327 |
GOF, S | 0.936 |
R1 [I>2σ(I)]a | 0.0673 |
wR2 [I>2σ(I)]b | 0.2347 |
Notes: (a) R1 = Σ||Fo| -
|Fc||/Σ|Fo|;
(b) wR2 = {Σ[w(Fo2 -
Fc2)2]/Σ[w(Fo2)2]}1/2.
Computer program(s): SHELXTL (Sheldrick, 2008);
SHELXL2014 (Sheldrick, 2015). |
Bond-valence-sum (BVS)a analysis for PTC-54 topNote: (a) Vi =ΣSij = Σexp[(r0 -
rij)/B], where r0 is the length of a single bond (here
r0 = 1.815 Å for the Tiiv—O bond), rij is the bond
length between atoms i and j (expressed in Å); B is a constant,
which is about 0.37 Å in this work; Vi is the sum of all bond
valences of the bonds formed by a given atom i (Palenik,
2003; Brown, 2009). |
Ti1 | 4.254 | | Ti2 | 3.921 | |
Ti1—O2 | 0.729 | d = 1.908 (2) | Ti2—O16 | 1.033 | d = 1.779 (3) |
Ti1—O2 | 0.729 | d = 1.908 (2) | Ti2—O1 | 0.638 | d = 1.957 (2) |
Ti1—O11 | 0.700 | d = 1.923 (2) | Ti2—O4 | 0.611 | d = 1.973 (2) |
Ti1—O11 | 0.700 | d = 1.923 (2) | Ti2—O10 | 0.600 | d = 1.980 (2) |
Ti1—O5 | 0.698 | d = 1.924 (2) | Ti2—O14 | 0.524 | d = 2.030 (3) |
Ti1—O5 | 0.698 | d = 1.924 (2) | Ti2—O13 | 0.514 | d = 2.037 (3) |
| | | | | |
Ti3 | 3.949 | | Ti4 | 3.952 | |
Ti3—O18 | 1.053 | d = 1.772 (3) | Ti4—O12 | 1.050 | d = 1.773 (3) |
Ti3—O1 | 0.630 | d = 1.962 (2) | Ti4—O1 | 0.645 | d = 1.953 (2) |
Ti3—O7 | 0.621 | d = 1.967 (3) | Ti4—O8 | 0.611 | d = 1.973 (2) |
Ti3—O6 | 0.615 | d = 1.971 (3) | Ti4—O3 | 0.608 | d = 1.975 (3) |
Ti3—O13 | 0.524 | d = 2.030 (3) | Ti4—O14 | 0.516 | d = 2.036 (3) |
Ti3—O9 | 0.506 | d = 2.043 (3) | Ti4—O9 | 0.521 | d = 2.032 (3) |
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