The title compound, [Hf(C11H19O2)3(NO3)], is a mixed-ligand MOCVD precursor. Hf has distorted square antiprismatic coordination. Of the six tert-butyl groups present, four are found to be disordered.
Supporting information
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).
Nitratotris(2,2,6,6-tetramethyl-3,5-heptadionato)hafnium(IV)
top
Crystal data top
[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 | |
Data collection top
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 top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.061 | 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 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | 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) |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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) | | |