Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680202202X/cf6224sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680202202X/cf6224Isup2.hkl |
CCDC reference: 202965
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.012 Å
- R factor = 0.061
- wR factor = 0.137
- Data-to-parameter ratio = 18.2
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level B:
PLAT_213 Alert B Atom C17A has ADP max/min Ratio ........... 4.70 prolate
Author response: The atoms C17A is a part of one of the four disordered tertiary butyl groups and has a high ADP max/min ratio. We have tried to resolve this disorder by assigning alternative positions with partial occupancies for all the four t-butyl groups but some of the atoms continue to have high ADP max/min ratio. This is could be indicative of the dynamic nature of the disorder in these groups. |
PLAT_213 Alert B Atom C17B has ADP max/min Ratio ........... 4.70 prolate
Author response: The atoms C17A is a part of one of the four disordered tertiary butyl groups and has a high ADP max/min ratio. We have tried to resolve this disorder by assigning alternative positions with partial occupancies for all the four t-butyl groups but some of the atoms continue to have high ADP max/min ratio. This is could be indicative of the dynamic nature of the disorder in these groups. |
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.438 0.538 Tmin and Tmax expected: 0.324 0.538 RR = 1.352 Please check that your absorption correction is appropriate. REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.63 From the CIF: _reflns_number_total 8429 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 9170 Completeness (_total/calc) 91.92% Alert C: < 95% complete PLAT_213 Alert C Atom C28A has ADP max/min Ratio ........... 3.10 prolate PLAT_213 Alert C Atom C29A has ADP max/min Ratio ........... 3.40 prolate PLAT_213 Alert C Atom C32A has ADP max/min Ratio ........... 3.10 prolate PLAT_213 Alert C Atom C28B has ADP max/min Ratio ........... 3.10 prolate PLAT_213 Alert C Atom C29B has ADP max/min Ratio ........... 3.40 prolate PLAT_213 Alert C Atom C32B has ADP max/min Ratio ........... 3.10 prolate
0 Alert Level A = Potentially serious problem
2 Alert Level B = Potential problem
8 Alert Level C = Please check
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998; data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Hf(C11H19O2)3(NO3)] | Z = 2 |
Mr = 790.29 | F(000) = 812 |
Triclinic, P1 | Dx = 1.333 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.156 (9) Å | Cell parameters from 21660 reflections |
b = 10.590 (9) Å | θ = 1.1–27.6° |
c = 19.277 (17) Å | µ = 2.70 mm−1 |
α = 79.683 (16)° | T = 293 K |
β = 75.336 (16)° | Prism, pale yellow |
γ = 83.579 (16)° | 0.52 × 0.36 × 0.23 mm |
V = 1969 (3) Å3 |
Bruker SMART CCD area-detector diffractometer | 8429 independent reflections |
Radiation source: fine-focus sealed tube | 4904 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.092 |
ω scans | θmax = 27.6°, θmin = 1.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.438, Tmax = 0.538 | k = −13→13 |
21660 measured reflections | l = −24→25 |
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)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 0.92 | w = 1/[σ2(Fo2) + (0.0539P)2] where P = (Fo2 + 2Fc2)/3 |
8429 reflections | (Δ/σ)max = 0.013 |
463 parameters | Δρmax = 0.82 e Å−3 |
0 restraints | Δρmin = −0.51 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Hf1 | 0.96556 (4) | 0.58509 (4) | 0.75306 (2) | 0.04918 (14) | |
O4 | 0.8145 (4) | 0.6887 (5) | 0.8258 (2) | 0.0393 (12) | |
O6 | 1.1614 (5) | 0.5069 (5) | 0.7674 (3) | 0.0422 (13) | |
O1 | 1.0897 (5) | 0.5887 (5) | 0.6454 (3) | 0.0452 (13) | |
O5 | 0.9244 (5) | 0.4641 (5) | 0.8563 (3) | 0.0414 (12) | |
O3 | 1.0636 (5) | 0.7482 (5) | 0.7549 (3) | 0.0435 (13) | |
O2 | 0.8556 (5) | 0.7170 (5) | 0.6844 (3) | 0.0491 (14) | |
O7 | 0.9655 (5) | 0.3804 (5) | 0.7236 (3) | 0.0561 (15) | |
O8 | 0.7760 (5) | 0.4849 (5) | 0.7536 (3) | 0.0548 (15) | |
C23 | 0.9875 (7) | 0.3786 (7) | 0.8909 (4) | 0.0402 (18) | |
C12 | 1.0243 (8) | 0.8603 (8) | 0.7695 (4) | 0.0445 (19) | |
C1 | 1.0885 (8) | 0.6402 (8) | 0.5817 (4) | 0.046 (2) | |
C14 | 0.7957 (7) | 0.8032 (8) | 0.8355 (4) | 0.0432 (19) | |
C25 | 1.2088 (7) | 0.4218 (7) | 0.8099 (4) | 0.0390 (18) | |
C24 | 1.1247 (7) | 0.3531 (7) | 0.8713 (4) | 0.046 (2) | |
H24 | 1.1649 | 0.2873 | 0.8997 | 0.055* | |
C13 | 0.8949 (8) | 0.8917 (8) | 0.8069 (4) | 0.054 (2) | |
H13 | 0.8717 | 0.9768 | 0.8137 | 0.065* | |
C3 | 0.8710 (8) | 0.7608 (7) | 0.6185 (5) | 0.049 (2) | |
C26 | 1.3634 (7) | 0.4019 (8) | 0.7909 (4) | 0.047 (2) | |
C30 | 0.8977 (8) | 0.3043 (8) | 0.9599 (5) | 0.055 (2) | |
C15 | 0.6574 (8) | 0.8389 (8) | 0.8829 (5) | 0.053 (2) | |
C19 | 1.1355 (8) | 0.9560 (8) | 0.7403 (5) | 0.057 (2) | |
C8 | 1.2125 (9) | 0.6052 (9) | 0.5225 (4) | 0.059 (2) | |
C4 | 0.7556 (8) | 0.8522 (8) | 0.6000 (4) | 0.054 (2) | |
C2 | 0.9852 (8) | 0.7246 (8) | 0.5658 (4) | 0.055 (2) | |
H2 | 0.9906 | 0.7601 | 0.5175 | 0.066* | |
C10 | 1.2434 (11) | 0.4648 (11) | 0.5369 (6) | 0.098 (4) | |
H10A | 1.1693 | 0.4214 | 0.5316 | 0.146* | |
H10B | 1.2552 | 0.4406 | 0.5855 | 0.146* | |
H10C | 1.3256 | 0.4412 | 0.5031 | 0.146* | |
C9 | 1.3297 (10) | 0.6721 (12) | 0.5284 (6) | 0.108 (4) | |
H9A | 1.4097 | 0.6497 | 0.4927 | 0.162* | |
H9B | 1.346 | 0.6463 | 0.576 | 0.162* | |
H9C | 1.3091 | 0.7635 | 0.5202 | 0.162* | |
C5 | 0.6268 (10) | 0.7804 (11) | 0.6250 (6) | 0.101 (4) | |
H5A | 0.6014 | 0.764 | 0.6771 | 0.151* | |
H5B | 0.6428 | 0.7002 | 0.6066 | 0.151* | |
H5C | 0.5545 | 0.8314 | 0.6072 | 0.151* | |
C6 | 0.7696 (11) | 0.8988 (11) | 0.5194 (5) | 0.104 (4) | |
H6A | 0.6871 | 0.947 | 0.512 | 0.155* | |
H6B | 0.7859 | 0.8262 | 0.4941 | 0.155* | |
H6C | 0.8447 | 0.9528 | 0.5011 | 0.155* | |
C11 | 1.1911 (12) | 0.6345 (13) | 0.4482 (5) | 0.116 (5) | |
H11A | 1.2648 | 0.594 | 0.4158 | 0.174* | |
H11B | 1.1879 | 0.7259 | 0.4328 | 0.174* | |
H11C | 1.1065 | 0.6027 | 0.4477 | 0.174* | |
C7 | 0.7438 (12) | 0.9616 (10) | 0.6393 (6) | 0.106 (4) | |
H7A | 0.7405 | 0.9301 | 0.6896 | 0.159* | |
H7B | 0.6619 | 1.0142 | 0.6352 | 0.159* | |
H7C | 0.8214 | 1.012 | 0.6188 | 0.159* | |
O9 | 0.7787 (6) | 0.2891 (6) | 0.7351 (4) | 0.0746 (19) | |
N1 | 0.8370 (7) | 0.3806 (7) | 0.7373 (4) | 0.0500 (17) | |
C16A | 0.625 (13) | 0.988 (14) | 0.882 (7) | 0.15 (4) | 0.55 (5) |
H16A | 0.5282 | 1.0073 | 0.8892 | 0.231* | 0.55 (5) |
H16B | 0.6703 | 1.0326 | 0.8355 | 0.231* | 0.55 (5) |
H16C | 0.6562 | 1.0138 | 0.9195 | 0.231* | 0.55 (5) |
C17A | 0.648 (8) | 0.781 (10) | 0.957 (4) | 0.18 (4) | 0.55 (5) |
H17A | 0.5686 | 0.8174 | 0.9873 | 0.27* | 0.55 (5) |
H17B | 0.728 | 0.7962 | 0.9711 | 0.27* | 0.55 (5) |
H17C | 0.6415 | 0.6898 | 0.9613 | 0.27* | 0.55 (5) |
C18A | 0.548 (5) | 0.808 (6) | 0.852 (3) | 0.098 (11) | 0.55 (5) |
H18A | 0.5599 | 0.7189 | 0.8462 | 0.147* | 0.55 (5) |
H18B | 0.5514 | 0.8608 | 0.8058 | 0.147* | 0.55 (5) |
H18C | 0.4608 | 0.8239 | 0.8843 | 0.147* | 0.55 (5) |
C16B | 0.602 (17) | 0.970 (17) | 0.851 (9) | 0.15 (4) | 0.45 (5) |
H16D | 0.5491 | 1.0145 | 0.8892 | 0.231* | 0.45 (5) |
H16E | 0.5444 | 0.9589 | 0.8198 | 0.231* | 0.45 (5) |
H16F | 0.676 | 1.0202 | 0.8228 | 0.231* | 0.45 (5) |
C17B | 0.679 (10) | 0.864 (11) | 0.951 (5) | 0.18 (4) | 0.45 (5) |
H17D | 0.6461 | 0.7959 | 0.9892 | 0.27* | 0.45 (5) |
H17E | 0.6309 | 0.9442 | 0.9621 | 0.27* | 0.45 (5) |
H17F | 0.7749 | 0.8696 | 0.9461 | 0.27* | 0.45 (5) |
C18B | 0.559 (6) | 0.750 (6) | 0.882 (3) | 0.098 (11) | 0.45 (5) |
H18D | 0.5702 | 0.6722 | 0.9147 | 0.147* | 0.45 (5) |
H18E | 0.5727 | 0.7311 | 0.8338 | 0.147* | 0.45 (5) |
H18F | 0.4681 | 0.7889 | 0.8971 | 0.147* | 0.45 (5) |
C20A | 1.219 (3) | 0.925 (2) | 0.6636 (10) | 0.101 (7) | 0.595 (12) |
H20A | 1.2744 | 0.9953 | 0.639 | 0.151* | 0.595 (12) |
H20B | 1.1571 | 0.9141 | 0.6353 | 0.151* | 0.595 (12) |
H20C | 1.2766 | 0.8478 | 0.6697 | 0.151* | 0.595 (12) |
C21A | 1.087 (3) | 1.093 (2) | 0.7326 (18) | 0.129 (14) | 0.595 (12) |
H21A | 1.0559 | 1.1185 | 0.7798 | 0.194* | 0.595 (12) |
H21B | 1.0139 | 1.1068 | 0.7085 | 0.194* | 0.595 (12) |
H21C | 1.161 | 1.1441 | 0.7045 | 0.194* | 0.595 (12) |
C22A | 1.246 (2) | 0.916 (2) | 0.7845 (12) | 0.101 (7) | 0.595 (12) |
H22A | 1.2728 | 0.8261 | 0.7846 | 0.151* | 0.595 (12) |
H22B | 1.2087 | 0.9312 | 0.8336 | 0.151* | 0.595 (12) |
H22C | 1.3233 | 0.9655 | 0.7629 | 0.151* | 0.595 (12) |
C20B | 1.119 (4) | 1.018 (4) | 0.6668 (15) | 0.101 (7) | 0.405 (12) |
H20D | 1.2004 | 1.0593 | 0.6405 | 0.151* | 0.405 (12) |
H20E | 1.0427 | 1.0803 | 0.6717 | 0.151* | 0.405 (12) |
H20F | 1.1038 | 0.9533 | 0.641 | 0.151* | 0.405 (12) |
C21B | 1.111 (4) | 1.060 (4) | 0.788 (3) | 0.129 (14) | 0.405 (12) |
H21D | 1.1637 | 1.0373 | 0.8239 | 0.194* | 0.405 (12) |
H21E | 1.0155 | 1.0673 | 0.8121 | 0.194* | 0.405 (12) |
H21F | 1.1366 | 1.1405 | 0.7588 | 0.194* | 0.405 (12) |
C22B | 1.265 (4) | 0.901 (4) | 0.733 (2) | 0.101 (7) | 0.405 (12) |
H22D | 1.2767 | 0.8321 | 0.7053 | 0.151* | 0.405 (12) |
H22E | 1.2795 | 0.8668 | 0.7806 | 0.151* | 0.405 (12) |
H22F | 1.3287 | 0.9639 | 0.7093 | 0.151* | 0.405 (12) |
C27A | 1.415 (3) | 0.402 (4) | 0.7100 (16) | 0.108 (11) | 0.557 (16) |
H27A | 1.5125 | 0.3902 | 0.6979 | 0.163* | 0.557 (16) |
H27B | 1.3868 | 0.4827 | 0.6842 | 0.163* | 0.557 (16) |
H27C | 1.3774 | 0.3333 | 0.6964 | 0.163* | 0.557 (16) |
C28A | 1.415 (2) | 0.509 (3) | 0.818 (2) | 0.125 (12) | 0.557 (16) |
H28A | 1.5014 | 0.4807 | 0.8298 | 0.187* | 0.557 (16) |
H28B | 1.3505 | 0.5305 | 0.8612 | 0.187* | 0.557 (16) |
H28C | 1.426 | 0.584 | 0.7815 | 0.187* | 0.557 (16) |
C29A | 1.414 (2) | 0.273 (3) | 0.8263 (18) | 0.115 (11) | 0.557 (16) |
H29A | 1.4182 | 0.2094 | 0.7955 | 0.172* | 0.557 (16) |
H29B | 1.352 | 0.2477 | 0.8723 | 0.172* | 0.557 (16) |
H29C | 1.5028 | 0.2784 | 0.8335 | 0.172* | 0.557 (16) |
C27B | 1.408 (4) | 0.323 (5) | 0.735 (2) | 0.108 (11) | 0.443 (16) |
H27D | 1.5035 | 0.3295 | 0.7142 | 0.163* | 0.443 (16) |
H27E | 1.3583 | 0.3514 | 0.6979 | 0.163* | 0.443 (16) |
H27F | 1.3905 | 0.2351 | 0.7554 | 0.163* | 0.443 (16) |
C28B | 1.426 (3) | 0.523 (4) | 0.756 (3) | 0.125 (12) | 0.443 (16) |
H28D | 1.518 | 0.504 | 0.7295 | 0.187* | 0.443 (16) |
H28E | 1.4273 | 0.5736 | 0.7922 | 0.187* | 0.443 (16) |
H28F | 1.3745 | 0.5695 | 0.723 | 0.187* | 0.443 (16) |
C29B | 1.425 (3) | 0.356 (4) | 0.853 (2) | 0.115 (11) | 0.443 (16) |
H29D | 1.4285 | 0.2634 | 0.863 | 0.172* | 0.443 (16) |
H29E | 1.3702 | 0.3896 | 0.8952 | 0.172* | 0.443 (16) |
H29F | 1.5153 | 0.3839 | 0.8423 | 0.172* | 0.443 (16) |
C31A | 0.808 (6) | 0.226 (3) | 0.937 (4) | 0.107 (12) | 0.569 (18) |
H31A | 0.7395 | 0.1916 | 0.978 | 0.161* | 0.569 (18) |
H31B | 0.8619 | 0.1559 | 0.915 | 0.161* | 0.569 (18) |
H31C | 0.7645 | 0.2786 | 0.9017 | 0.161* | 0.569 (18) |
C32A | 0.800 (3) | 0.402 (3) | 1.0031 (14) | 0.106 (11) | 0.569 (18) |
H32A | 0.7433 | 0.356 | 1.0457 | 0.159* | 0.569 (18) |
H32B | 0.744 | 0.451 | 0.9732 | 0.159* | 0.569 (18) |
H32C | 0.8527 | 0.4584 | 1.0172 | 0.159* | 0.569 (18) |
C33A | 0.983 (3) | 0.213 (3) | 1.0053 (17) | 0.118 (12) | 0.569 (18) |
H33A | 1.0001 | 0.2559 | 1.0418 | 0.177* | 0.569 (18) |
H33B | 1.0689 | 0.188 | 0.9744 | 0.177* | 0.569 (18) |
H33C | 0.9351 | 0.1378 | 1.0283 | 0.177* | 0.569 (18) |
C31B | 0.769 (9) | 0.279 (5) | 0.938 (5) | 0.107 (12) | 0.431 (18) |
H31D | 0.7255 | 0.2087 | 0.9718 | 0.161* | 0.431 (18) |
H31E | 0.7931 | 0.2583 | 0.8902 | 0.161* | 0.431 (18) |
H31F | 0.7072 | 0.3548 | 0.94 | 0.161* | 0.431 (18) |
C32B | 0.892 (4) | 0.363 (3) | 1.0186 (15) | 0.106 (11) | 0.431 (18) |
H32D | 0.942 | 0.4392 | 1.003 | 0.159* | 0.431 (18) |
H32E | 0.9308 | 0.3053 | 1.0536 | 0.159* | 0.431 (18) |
H32F | 0.7984 | 0.3871 | 1.0404 | 0.159* | 0.431 (18) |
C33B | 0.955 (5) | 0.164 (4) | 0.9735 (18) | 0.118 (12) | 0.431 (18) |
H33D | 0.961 | 0.1422 | 1.0232 | 0.177* | 0.431 (18) |
H33E | 1.0445 | 0.1549 | 0.9422 | 0.177* | 0.431 (18) |
H33F | 0.8962 | 0.1087 | 0.9637 | 0.177* | 0.431 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hf1 | 0.0400 (2) | 0.0499 (2) | 0.0505 (2) | 0.00272 (14) | −0.00398 (15) | −0.00246 (16) |
O4 | 0.033 (3) | 0.043 (3) | 0.034 (3) | −0.001 (2) | 0.006 (2) | −0.005 (2) |
O6 | 0.030 (3) | 0.044 (3) | 0.044 (3) | 0.000 (2) | −0.003 (2) | 0.007 (3) |
O1 | 0.040 (3) | 0.050 (3) | 0.036 (3) | 0.011 (2) | −0.001 (2) | −0.004 (3) |
O5 | 0.032 (3) | 0.046 (3) | 0.038 (3) | −0.001 (2) | −0.003 (2) | 0.006 (2) |
O3 | 0.032 (3) | 0.042 (3) | 0.053 (3) | −0.002 (2) | −0.002 (2) | −0.009 (3) |
O2 | 0.045 (3) | 0.059 (3) | 0.036 (3) | 0.012 (3) | −0.010 (3) | 0.000 (3) |
O7 | 0.044 (3) | 0.047 (3) | 0.073 (4) | −0.003 (3) | 0.001 (3) | −0.020 (3) |
O8 | 0.037 (3) | 0.054 (4) | 0.076 (4) | 0.003 (3) | −0.021 (3) | −0.011 (3) |
C23 | 0.037 (4) | 0.041 (5) | 0.043 (5) | −0.015 (4) | −0.007 (4) | −0.003 (4) |
C12 | 0.050 (5) | 0.042 (5) | 0.044 (5) | −0.008 (4) | −0.016 (4) | −0.004 (4) |
C1 | 0.042 (5) | 0.051 (5) | 0.040 (5) | −0.006 (4) | −0.002 (4) | −0.005 (4) |
C14 | 0.039 (4) | 0.058 (5) | 0.034 (5) | 0.004 (4) | −0.009 (3) | −0.016 (4) |
C25 | 0.037 (4) | 0.039 (4) | 0.044 (5) | 0.003 (3) | −0.010 (4) | −0.016 (4) |
C24 | 0.043 (5) | 0.045 (5) | 0.046 (5) | −0.002 (4) | −0.019 (4) | 0.011 (4) |
C13 | 0.055 (5) | 0.047 (5) | 0.061 (6) | 0.005 (4) | −0.001 (4) | −0.031 (4) |
C3 | 0.047 (5) | 0.046 (5) | 0.055 (6) | 0.002 (4) | −0.018 (4) | −0.005 (4) |
C26 | 0.030 (4) | 0.048 (5) | 0.054 (5) | 0.003 (4) | −0.006 (4) | 0.003 (4) |
C30 | 0.052 (5) | 0.057 (5) | 0.049 (6) | −0.012 (4) | −0.007 (4) | 0.012 (4) |
C15 | 0.041 (5) | 0.065 (6) | 0.053 (6) | 0.005 (4) | −0.002 (4) | −0.028 (5) |
C19 | 0.041 (5) | 0.046 (5) | 0.082 (7) | −0.005 (4) | −0.008 (5) | −0.011 (5) |
C8 | 0.052 (5) | 0.080 (7) | 0.039 (5) | 0.010 (5) | −0.003 (4) | −0.013 (5) |
C4 | 0.053 (5) | 0.062 (6) | 0.041 (5) | 0.013 (4) | −0.014 (4) | −0.003 (4) |
C2 | 0.054 (5) | 0.073 (6) | 0.029 (4) | 0.005 (4) | −0.004 (4) | 0.007 (4) |
C10 | 0.077 (7) | 0.124 (10) | 0.087 (8) | 0.017 (7) | 0.004 (6) | −0.053 (8) |
C9 | 0.058 (7) | 0.146 (11) | 0.108 (10) | −0.011 (7) | 0.012 (6) | −0.032 (8) |
C5 | 0.076 (8) | 0.103 (9) | 0.116 (10) | 0.025 (7) | −0.040 (7) | 0.005 (7) |
C6 | 0.094 (8) | 0.132 (10) | 0.066 (7) | 0.048 (7) | −0.027 (6) | 0.011 (7) |
C11 | 0.096 (9) | 0.178 (13) | 0.053 (7) | 0.030 (8) | 0.008 (6) | −0.021 (8) |
C7 | 0.133 (10) | 0.087 (8) | 0.111 (10) | 0.052 (7) | −0.070 (8) | −0.031 (7) |
O9 | 0.062 (4) | 0.068 (4) | 0.105 (6) | −0.016 (3) | −0.025 (4) | −0.029 (4) |
N1 | 0.046 (4) | 0.057 (5) | 0.049 (4) | −0.006 (4) | −0.016 (3) | −0.007 (4) |
C16A | 0.10 (5) | 0.11 (4) | 0.21 (12) | 0.03 (3) | 0.05 (6) | −0.05 (5) |
C17A | 0.07 (3) | 0.36 (12) | 0.048 (14) | 0.07 (5) | 0.031 (18) | 0.02 (5) |
C18A | 0.052 (10) | 0.14 (4) | 0.10 (3) | 0.00 (2) | 0.00 (2) | −0.04 (2) |
C16B | 0.10 (5) | 0.11 (4) | 0.21 (12) | 0.03 (3) | 0.05 (6) | −0.05 (5) |
C17B | 0.07 (3) | 0.36 (12) | 0.048 (14) | 0.07 (5) | 0.031 (18) | 0.02 (5) |
C18B | 0.052 (10) | 0.14 (4) | 0.10 (3) | 0.00 (2) | 0.00 (2) | −0.04 (2) |
C20A | 0.127 (19) | 0.100 (16) | 0.063 (9) | −0.065 (12) | 0.002 (13) | 0.019 (12) |
C21A | 0.076 (13) | 0.052 (14) | 0.23 (4) | −0.020 (10) | 0.01 (2) | 0.004 (18) |
C22A | 0.111 (13) | 0.102 (13) | 0.103 (19) | −0.049 (11) | −0.041 (18) | −0.004 (16) |
C20B | 0.127 (19) | 0.100 (16) | 0.063 (9) | −0.065 (12) | 0.002 (13) | 0.019 (12) |
C21B | 0.076 (13) | 0.052 (14) | 0.23 (4) | −0.020 (10) | 0.01 (2) | 0.004 (18) |
C22B | 0.111 (13) | 0.102 (13) | 0.103 (19) | −0.049 (11) | −0.041 (18) | −0.004 (16) |
C27A | 0.046 (8) | 0.19 (4) | 0.07 (2) | 0.04 (2) | −0.010 (12) | −0.003 (17) |
C28A | 0.026 (7) | 0.128 (15) | 0.23 (4) | −0.004 (8) | −0.01 (2) | −0.08 (3) |
C29A | 0.024 (7) | 0.11 (2) | 0.16 (3) | 0.014 (14) | 0.009 (11) | 0.040 (19) |
C27B | 0.046 (8) | 0.19 (4) | 0.07 (2) | 0.04 (2) | −0.010 (12) | −0.003 (17) |
C28B | 0.026 (7) | 0.128 (15) | 0.23 (4) | −0.004 (8) | −0.01 (2) | −0.08 (3) |
C29B | 0.024 (7) | 0.11 (2) | 0.16 (3) | 0.014 (14) | 0.009 (11) | 0.040 (19) |
C31A | 0.11 (4) | 0.08 (3) | 0.100 (11) | −0.04 (3) | 0.04 (2) | 0.01 (3) |
C32A | 0.13 (2) | 0.096 (17) | 0.058 (13) | −0.049 (18) | 0.053 (17) | −0.012 (12) |
C33A | 0.082 (17) | 0.14 (3) | 0.09 (2) | −0.027 (15) | −0.001 (14) | 0.072 (18) |
C31B | 0.11 (4) | 0.08 (3) | 0.100 (11) | −0.04 (3) | 0.04 (2) | 0.01 (3) |
C32B | 0.13 (2) | 0.096 (17) | 0.058 (13) | −0.049 (18) | 0.053 (17) | −0.012 (12) |
C33B | 0.082 (17) | 0.14 (3) | 0.09 (2) | −0.027 (15) | −0.001 (14) | 0.072 (18) |
Hf1—O3 | 2.098 (5) | C26—C28B | 1.47 (4) |
Hf1—O6 | 2.132 (5) | C26—C29B | 1.47 (4) |
Hf1—O1 | 2.134 (5) | C26—C29A | 1.51 (3) |
Hf1—O5 | 2.136 (5) | C26—C27A | 1.51 (3) |
Hf1—O4 | 2.147 (5) | C26—C28A | 1.53 (3) |
Hf1—O2 | 2.165 (5) | C30—C32B | 1.37 (3) |
Hf1—O8 | 2.297 (5) | C30—C31A | 1.50 (7) |
Hf1—O7 | 2.337 (5) | C30—C31B | 1.53 (11) |
Hf1—N1 | 2.748 (8) | C30—C33B | 1.53 (4) |
O4—C14 | 1.246 (8) | C30—C33A | 1.54 (3) |
O6—C25 | 1.247 (8) | C30—C32A | 1.55 (2) |
O1—C1 | 1.253 (9) | C15—C17A | 1.43 (8) |
O5—C23 | 1.244 (8) | C15—C18B | 1.45 (7) |
O3—C12 | 1.267 (8) | C15—C17B | 1.46 (13) |
O2—C3 | 1.248 (9) | C15—C18A | 1.48 (5) |
O7—N1 | 1.263 (8) | C15—C16B | 1.5 (2) |
O8—N1 | 1.254 (8) | C15—C16A | 1.57 (13) |
C23—C24 | 1.358 (10) | C19—C22B | 1.36 (4) |
C23—C30 | 1.546 (10) | C19—C21A | 1.48 (3) |
C12—C13 | 1.365 (10) | C19—C20B | 1.49 (3) |
C12—C19 | 1.532 (11) | C19—C21B | 1.52 (5) |
C1—C2 | 1.360 (10) | C19—C22A | 1.55 (2) |
C1—C8 | 1.532 (10) | C19—C20A | 1.58 (2) |
C14—C13 | 1.394 (11) | C8—C11 | 1.475 (12) |
C14—C15 | 1.519 (10) | C8—C10 | 1.475 (13) |
C25—C24 | 1.407 (10) | C8—C9 | 1.490 (13) |
C25—C26 | 1.519 (10) | C4—C7 | 1.473 (12) |
C3—C2 | 1.403 (10) | C4—C5 | 1.515 (13) |
C3—C4 | 1.506 (10) | C4—C6 | 1.519 (12) |
C26—C27B | 1.43 (5) | O9—N1 | 1.204 (8) |
O3—Hf1—O6 | 76.81 (19) | C25—C26—C28A | 106.1 (11) |
O3—Hf1—O1 | 85.63 (19) | C32B—C30—C31A | 137 (3) |
O6—Hf1—O1 | 75.40 (19) | C32B—C30—C31B | 122 (3) |
O3—Hf1—O5 | 111.9 (2) | C31A—C30—C31B | 25 (2) |
O6—Hf1—O5 | 75.42 (18) | C32B—C30—C33B | 110.0 (19) |
O1—Hf1—O5 | 141.04 (18) | C31A—C30—C33B | 74 (2) |
O3—Hf1—O4 | 76.85 (19) | C31B—C30—C33B | 98 (2) |
O6—Hf1—O4 | 126.77 (19) | C32B—C30—C33A | 75 (2) |
O1—Hf1—O4 | 146.00 (18) | C31A—C30—C33A | 108 (2) |
O5—Hf1—O4 | 72.95 (19) | C31B—C30—C33A | 129 (3) |
O3—Hf1—O2 | 84.3 (2) | C33B—C30—C33A | 37.2 (15) |
O6—Hf1—O2 | 145.59 (19) | C32B—C30—C23 | 109.7 (15) |
O1—Hf1—O2 | 74.68 (19) | C31A—C30—C23 | 108 (2) |
O5—Hf1—O2 | 138.87 (19) | C31B—C30—C23 | 106 (3) |
O4—Hf1—O2 | 74.78 (19) | C33B—C30—C23 | 110.5 (17) |
O3—Hf1—O8 | 152.09 (19) | C33A—C30—C23 | 112.0 (13) |
O6—Hf1—O8 | 130.6 (2) | C32B—C30—C32A | 42.2 (14) |
O1—Hf1—O8 | 104.6 (2) | C31A—C30—C32A | 105.8 (19) |
O5—Hf1—O8 | 76.35 (19) | C31B—C30—C32A | 84 (2) |
O4—Hf1—O8 | 80.7 (2) | C33B—C30—C32A | 138.2 (18) |
O2—Hf1—O8 | 73.9 (2) | C33A—C30—C32A | 113.3 (17) |
O3—Hf1—O7 | 152.26 (19) | C23—C30—C32A | 109.1 (11) |
O6—Hf1—O7 | 80.2 (2) | C17A—C15—C18B | 86 (4) |
O1—Hf1—O7 | 73.61 (19) | C17A—C15—C17B | 38 (7) |
O5—Hf1—O7 | 76.5 (2) | C18B—C15—C17B | 121 (4) |
O4—Hf1—O7 | 130.17 (18) | C17A—C15—C18A | 114 (4) |
O2—Hf1—O7 | 106.9 (2) | C18B—C15—C18A | 31 (2) |
O8—Hf1—O7 | 54.15 (19) | C17B—C15—C18A | 140 (4) |
O3—Hf1—N1 | 174.65 (19) | C17A—C15—C14 | 111 (3) |
O6—Hf1—N1 | 105.4 (2) | C18B—C15—C14 | 110 (3) |
O1—Hf1—N1 | 90.2 (2) | C17B—C15—C14 | 108 (4) |
O5—Hf1—N1 | 73.4 (2) | C18A—C15—C14 | 110 (2) |
O4—Hf1—N1 | 105.1 (2) | C17A—C15—C16B | 131 (6) |
O2—Hf1—N1 | 91.3 (2) | C18B—C15—C16B | 105 (6) |
O8—Hf1—N1 | 26.95 (17) | C17B—C15—C16B | 102 (6) |
O7—Hf1—N1 | 27.27 (18) | C18A—C15—C16B | 76 (6) |
C14—O4—Hf1 | 133.9 (5) | C14—C15—C16B | 110 (6) |
C25—O6—Hf1 | 137.7 (5) | C17A—C15—C16A | 108 (6) |
C1—O1—Hf1 | 139.5 (5) | C18B—C15—C16A | 124 (5) |
C23—O5—Hf1 | 137.1 (5) | C17B—C15—C16A | 75 (6) |
C12—O3—Hf1 | 135.0 (5) | C18A—C15—C16A | 101 (5) |
C3—O2—Hf1 | 137.8 (5) | C14—C15—C16A | 114 (5) |
N1—O7—Hf1 | 94.8 (4) | C16B—C15—C16A | 28 (8) |
N1—O8—Hf1 | 97.0 (4) | C22B—C19—C21A | 129.7 (19) |
O5—C23—C24 | 123.4 (7) | C22B—C19—C20B | 108 (2) |
O5—C23—C30 | 114.6 (6) | C21A—C19—C20B | 63.7 (17) |
C24—C23—C30 | 122.0 (7) | C22B—C19—C21B | 111 (2) |
O3—C12—C13 | 122.7 (7) | C21A—C19—C21B | 44.7 (17) |
O3—C12—C19 | 113.3 (7) | C20B—C19—C21B | 108 (2) |
C13—C12—C19 | 124.0 (7) | C22B—C19—C12 | 114.0 (16) |
O1—C1—C2 | 122.4 (7) | C21A—C19—C12 | 115.9 (11) |
O1—C1—C8 | 116.1 (7) | C20B—C19—C12 | 106.0 (13) |
C2—C1—C8 | 121.5 (7) | C21B—C19—C12 | 109.4 (16) |
O4—C14—C13 | 122.9 (7) | C22B—C19—C22A | 39.3 (15) |
O4—C14—C15 | 115.0 (7) | C21A—C19—C22A | 115.9 (16) |
C13—C14—C15 | 122.0 (7) | C20B—C19—C22A | 141.6 (16) |
O6—C25—C24 | 122.1 (7) | C21B—C19—C22A | 78.0 (19) |
O6—C25—C26 | 114.5 (7) | C12—C19—C22A | 107.3 (10) |
C24—C25—C26 | 123.4 (7) | C22B—C19—C20A | 61.0 (15) |
C23—C24—C25 | 122.9 (7) | C21A—C19—C20A | 108.5 (15) |
C12—C13—C14 | 123.7 (7) | C20B—C19—C20A | 51.1 (14) |
O2—C3—C2 | 122.3 (7) | C21B—C19—C20A | 141.5 (17) |
O2—C3—C4 | 114.7 (7) | C12—C19—C20A | 107.8 (9) |
C2—C3—C4 | 122.9 (8) | C22A—C19—C20A | 100.1 (14) |
C27B—C26—C28B | 102 (2) | C11—C8—C10 | 106.4 (9) |
C27B—C26—C29B | 112.5 (19) | C11—C8—C9 | 111.1 (9) |
C28B—C26—C29B | 105.1 (19) | C10—C8—C9 | 109.2 (9) |
C27B—C26—C29A | 73.3 (16) | C11—C8—C1 | 114.5 (8) |
C28B—C26—C29A | 134.9 (17) | C10—C8—C1 | 107.8 (7) |
C29B—C26—C29A | 44.4 (15) | C9—C8—C1 | 107.8 (7) |
C27B—C26—C27A | 35.0 (19) | C7—C4—C3 | 107.6 (7) |
C28B—C26—C27A | 69.9 (19) | C7—C4—C5 | 110.7 (9) |
C29B—C26—C27A | 133.3 (17) | C3—C4—C5 | 107.6 (7) |
C29A—C26—C27A | 105.4 (16) | C7—C4—C6 | 110.7 (9) |
C27B—C26—C25 | 110.0 (19) | C3—C4—C6 | 114.9 (7) |
C28B—C26—C25 | 111.1 (14) | C5—C4—C6 | 105.3 (8) |
C29B—C26—C25 | 115.0 (14) | C1—C2—C3 | 123.3 (7) |
C29A—C26—C25 | 112.4 (11) | O9—N1—O8 | 123.1 (7) |
C27A—C26—C25 | 109.6 (13) | O9—N1—O7 | 123.0 (7) |
C27B—C26—C28A | 139 (2) | O8—N1—O7 | 113.8 (7) |
C28B—C26—C28A | 45.7 (16) | O9—N1—Hf1 | 176.0 (6) |
C29B—C26—C28A | 66.4 (17) | O8—N1—Hf1 | 56.1 (4) |
C29A—C26—C28A | 109.5 (17) | O7—N1—Hf1 | 57.9 (4) |
C27A—C26—C28A | 114.0 (19) |
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