![[HTML version]](/e/graphics/htmlborder.gif)
![[PDF version]](/e/graphics/pdfborder.gif)
![[Article Abstract]](/e/graphics/abstractborder.gif)
![[CIF]](/e/graphics/cifborder.gif)
![[3d view]](/e/graphics/3dviewborder.gif)
![[Structure Factors]](/e/graphics/structurefactorsborder.gif)
![[Issue contents]](/e/graphics/issuecontentsborder.gif)
![[Buy article online]](/logos/buy.gif)
![[Contents scheme]](bt6813contents.gif)
Acta Cryst. (2006). E62, m465-m468 [ doi:10.1107/S1600536806004156 ]
Di-![[mu]](/logos/entities/mu_rmgif.gif)
-hydroxo-![[kappa]](/logos/entities/kappa_rmgif.gif)
4O:O-bis[aquatris(triphenylsilanolato-O)zirconium(IV)] toluene solvate
Online 8 February 2006
Key indicators
- Single-crystal X-ray study
- T = 183 K
- Mean
![[sigma]](http://journals.iucr.org/logos/entities/sigma_rmgif.gif)
(C-C) = 0.013 Å
- R factor = 0.039
- wR factor = 0.106
- Data-to-parameter ratio = 10.7
checkCIF/PLATON results
No syntax errors found
Datablock: tt586
Alert level A
THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.4941
| Author Response: The title compound is a minor product from a reaction and crystals
were obtained after a complicated procedure lasting several days. All
operations had to be performed under strict inert conditions in anhydrous
solvents, since it had to be sure that the only water source was the amount of
water added deliberately (cf. _publ_section_exptl_prep). The reaction as well
as the crystallisation were done several times and only once crystalline
material was obtained. The crystal was the best out of this badge, although it
was very small and did nor diffract very well. The data set was recorded some
years ago on a CAD4 diffractometer, so for the sake of time in combination with
a weakly diffracting crystal, the theta(max) value is quite small leading to
this problem as well as to several other level A, B and C alerts. Nevertheless,
there are more than 9000 observed reflections and the important parts of the
structure, i.e. the coordination spheres of the zirconium atoms, show a good
resolution. The phenyl substituents as well as the solvent molecule are not
improtant for the point that we would like to state with this strucure.
|
PLAT023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6]..... 20.56 Deg.
| Author Response: vide infra
|
PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 20.56 Deg.
| Author Response: vide infra
|
PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C101
| Author Response: vide infra
|
Alert level B
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.39 Ratio
| Author Response: Several of the phenyl substituents of the triphenylsilanolate
ligands might be more appropriatley resolved as disordered due to a rotation
around the carbon silicon bond. Nevertheless, this would even have worsened
the data parameter ratio, so we decided to refine only one conformation. This
is also the reason for a number of additional A, B and C level alerts.
|
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C71
| Author Response: vide infra
|
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C81
| Author Response: vide infra
|
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C67
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C97
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C100
PLAT420_ALERT_2_B D-H Without Acceptor O4 - H4O ... ?
| Author Response: The \m-hydroxo as well as the water ligands are situated in a
hydrophobic cavity built up by the big number of phenyl groups of the
triphenylsilanolato ligands.
|
PLAT420_ALERT_2_B D-H Without Acceptor O5 - H5A ... ?
| Author Response: The \m-hydroxo as well as the water ligands are situated in a
hydrophobic cavity built up by the big number of phenyl groups of the
triphenylsilanolato ligands.
|
PLAT420_ALERT_2_B D-H Without Acceptor O9 - H9O ... ?
| Author Response: The \m-hydroxo as well as the water ligands are situated in a
hydrophobic cavity built up by the big number of phenyl groups of the
triphenylsilanolato ligands.
|
PLAT420_ALERT_2_B D-H Without Acceptor O10 - H10B ... ?
| Author Response: The \m-hydroxo as well as the water ligands are situated in a
hydrophobic cavity built up by the big number of phenyl groups of the
triphenylsilanolato ligands.
|
Alert level C
PLAT213_ALERT_2_C Atom C101 has ADP max/min Ratio ............. 3.30 prolat
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.08 Ratio
| Author Response: Several of the phenyl substituents of the triphenylsilanolate
ligands might be more appropriatley resolved as disordered due to a rotation
around the carbon silicon bond. Nevertheless, this would even have worsened
the data parameter ratio, so we decided to refine only one conformation. This
is also the reason for a number of additional A, B and C level alerts.
|
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.66 Ratio
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zr2 - O9 .. 9.52 su
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C57
| Author Response: vide infra
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C65
| Author Response: vide infra
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C69
| Author Response: vide infra
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C72
| Author Response: vide infra
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C94
| Author Response: vide infra
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C95
| Author Response: vide infra
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C102
| Author Response: vide infra
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C107
| Author Response: vide infra
|
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Zr1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Zr2
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C70
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C79
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C113
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C109
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13
4 ALERT level A = In general: serious problem
10 ALERT level B = Potentially serious problem
19 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
26 ALERT type 2 Indicator that the structure model may be wrong or deficient
5 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Copyright © International Union of Crystallography
IUCr Webmaster