• No se han encontrado resultados

CAPITULO II MARCO TEÓRICO Y CONCEPTUAL

2. BASES TEÓRICAS

The  Schrödinger  equation  is  not  a  completely  correct  description  of  the  interaction  of   electrons  and  nuclei  as  it  ignores  effects  due  to  special  relativity.  The  Dirac  equation   is  a  relativistically  correct  equation  on  the  other  hand  and  the  Schrödinger  equation   can  be  understood  as  an  approximation  to  it  by  taking  the  speed  of  light  to  be  

infinite.2  Due  to  the  complexity  of  the  Dirac  equation  it  is  rarely  affordable  but  for  the  

smallest  molecules,  but  popular  approximations  to  it  have  been  derived  that  can   capture  most  of  the  effects  of  relativity.    

 

Relativistic  effects  are  known  to  become  important  to  account  for,  for  the  lower   transition  metal  rows,  but  are  often  ignored  for  the  1st  transition  metal  row  (copper  

being  an  exception).  Relativistic  effects  have  previously  been  shown  to  be  negligible   for  57Fe  EFG  tensors167  according  to  Zeroth-­‐Order  Regular  Approximation  (ZORA)  

168,169  calculations,  an  approximation  the  relativistic  Dirac  equation.  170,170170  Recent  

developments  in  Douglas-­‐Kroll-­‐Hess  relativistic  approximations171  that  correct  for  

the  picture-­‐change  effect  on  electric  field  gradients170  (an  artifact  arising  due  to  the  

mismatch  between  a  nonrelativistic  operator  being  used  with  a  quasirelativistic   wavefunction/density),  have  allowed  us  to  explore  this  issue  by  performing  Douglas-­‐ Kroll-­‐Hess  (DKH)  relativistic  calculations  using  the  Orca  code.147  

 

In  a  recent  study,  DKH  electric  field  gradients  were  calculated  for  the  hydrogen   halides.170  By  using  spin-­‐free  Dirac-­‐DFT  results  as  reference  values  for  the  molecule  

test  set,  the  convergence  and  performance  of  the  DKH  approximation  could  be  

systematically  explored.  The  dependence  of  the  results  on  the  n-­‐th  order  of  the  DKHn   Hamiltonian  as  well  as  the  order  of  the  picture-­‐change  correction  were  explored  and   it  was  found  that  DKH2  (second  order  DKH)  with  picture-­‐change  corrections  was  a   generally  accurate  approximation  to  capture  scalar  relativistic  effects  on  EFGs.  The   picture-­‐change  correction  was  found  to  be  crucial  for  accurate  EFG  calculations.    

We  carried  out  such  DKHn  calculations  (and  non-­‐relativistic  calculations  for  

comparison)  using  the  revTPSSh  functional  and  the  decontracted  def2-­‐QZVPP  basis   set  using  the  Orca  code.  DKHn  calculations  up  to  n=3  were  carried  out.  Calculations   were  carried  out  with  and  without  picture-­‐change  corrections.  The  DKH2  calculations   were  found  to  be  ~1.5  times  more  expensive  than  nonrelativistic  calculations  while   DKH3  calculations  (including  picture-­‐change  corrections)  were  ~1.7  times  more   expensive.  

 

Table  7  Decontracted  basis  EFG  calculations  with  the  revTPSSh  functional  and  different  relativistic   approximations:  Vzz  values  in  au,a  compared  to  gas-­‐phase  MW  data.  

Comp.   NRb   DKH1   DKH1-­‐pcc   DKH2   DKH2-­‐pcc   DKH3-­‐pcc     Exp.   18   -­‐0.355   -­‐0.358   -­‐0.362   -­‐0.358   -­‐0.362   -­‐0.362   -­‐0.344   19   -­‐0.353   -­‐0.372   -­‐0.378   -­‐0.372   -­‐0.378   -­‐0.378   -­‐0.217   20   0.586   0.589   0.588   0.589   0.588   0.588    0.570   21   -­‐0.871   -­‐0.880   -­‐0.880   -­‐0.880   -­‐0.880   -­‐0.880   -­‐0.877   22   -­‐1.226   -­‐1.201   -­‐1.203   -­‐1.203   -­‐1.204   -­‐1.204   -­‐1.182   23   -­‐0.532   -­‐0.520   -­‐0.534   -­‐0.520   -­‐0.535   -­‐0.535   -­‐0.356   24   -­‐0.303   -­‐0.317   -­‐0.320   -­‐0.317   -­‐0.319   -­‐0.319   -­‐0.390                   MAEd   0.068   0.064   0.067   0.064   0.067   0.067     MEd   -­‐0.037   -­‐0.038   -­‐0.042   -­‐0.038   -­‐0.042   -­‐0.042     MaxEd   0.176   0.164   0.178   0.164   0.179   0.179     Sloped   1.008   0.999   0.998   1.000   0.999   0.999     aGaussian-­‐style,  decontracted  def2-­‐QZVPP  basis  set  and  BP86/AE1  geometries.  

b  NR:  Non-­‐relativistic.  

c  Picture-­‐change  correction  used.  

dMean  absolute  error  (MAE),  mean  error  (ME),  maximum  error  (MaxE)  and  slope  from  a  linear  regression  of  

DFT  vs.  experimental  data.  

   

Table  7  shows  the  results  of  these  calculations.  The  results  reveal  that  there  is   sometimes  an  overestimation  of  relativistic  effects  when  not  including  the  picture   change  correction.  Overall,  the  picture-­‐change  corrected  relativistic  effect  is  rather   small  and  does  not  significantly  affect  the  mean  absolute  error  of  EFGs  for  our  test  set   (although  some  molecules  seem  to  be  more  sensitive  than  others).  This  suggests  that   relativistic  calculations  for  3d  transition  metal  EFGs  are  generally  not  needed  as  the   DFT  functional  error  will  overshadow  any  error  resulting  from  the  neglect  of  

relativistic  effects.    

3.3.4.  Summary  

 

1. The  electric  field  gradient  in  the  gas-­‐phase  does  not  seem  overly  sensitive  to   geometric  effects  (BP86/TPSS  geometry  optimisations  with  a  moderate  basis   set  (AE1)  seem  to  be  sufficient).  

2. There  is  a  strong  basis  set  dependence  and  normal  contracted  basis  sets  are   unreliable  for  EFG  computations.  In  order  to  minimise  basis  set  errors  in  EFG   calculations,  a  large  decontracted  quadruple-­‐zeta  basis  set  on  the  metal  atom   is  recommended,  while  much  smaller  (double-­‐zeta)  normal  contracted  basis   sets  can  be  used  for  the  ligand  atoms  with  good  accuracy.  

3. Relativistic  effects  on  EFGs  can  be  easily  checked  for  nowadays  as  the  

additional  computational  cost  is  not  excessive.  Relativistic  effects  seem  to  be   small  for  1st  transition  metal  row  EFGs  and  can  probably  be  ignored  for  the  

most  part.  

4. The  DFT  functional  is  the  greatest  source  of  uncertainty  in  these  calculations   and  most  likely  responsible  for  the  remaining  deviations  with  experiment.  The   (rev)TPSS  and  (rev)TPSSh  hybrid  functionals  seem  to  be  the  most  reliable   functionals  for  EFG  computations  of  3d  transion  metal  complexes.  

5. Finally  it  must  be  noted  that  this  test  set  of  EFGs  is  rather  small  and  any  error   in  the  experimental  coupling  constant  or  quadrupole  moment  can  significantly   skew  the  results.  The  experimental  quadrupole  coupling  constants  have  small   error  bars,  however,  some  of  the  quadrupole  moments  have  sizeable  

uncertainties,  e.g.  over  30  %  for  53Cr.    

Recently  a  new  quadrupole  moment  of  -­‐4.8  fm2  instead  of  -­‐5.2  fm2  has  been  

suggested  for  51V.172  We  note,  however,  that  using  this  value  for  Q  would  

increase  the  deviation  for  the  EFG  at  the  V  nucleus  for  all  tested  functionals  as   all  of  them  underestimate  the  absolute  value  for  this  EFG  while  the  new  Q   would  increase  the  absolute  value.  Hence,  this  would  affect  the  comparison   between  methods  very  little.  

6. Our  DFT  functional  recommendations  should  be  further  explored  in  the  future.   It  is  likely  that  test  sets  from  solid-­‐state  experiments  are  necessary  as  

microwave  NQCC  determinations  for  transtion  metal  complexes  are  few.  This   will  inevitably  require  reliable  methods  to  take  solid-­‐state  effects  into  account.    

 

Finally,  we  give  a  table  with  estimated  DFT  functional  errors  for  selected  first  

transition  metal  row  nuclides  (in  MHz)  based  on  the  computed  mean  absolute  errors   in  EFG  Vzz  values  in  Table  6  and  Eq.  49.  Later  we  will  compare  computed  and  

experimental  51V  and  59Co  NQCC  data  in  the  solid-­‐state  where  this  table  will  become  

useful.    

Table  8  Estimated  DFT  errors  for  NQCC  (in  MHz  )  of  the  first  transition  metal  row  nuclides  for  selected   functionals.a  

Comp.   B3LYP   PBE   TPSS   TPSSh   revTPSS   revTPSSh  

45Sc   6.0   5.0   4.2   4.2   3.8   3.5   47Ti   8.2   6.8   5.8   5.7   5.2   4.8   49Ti   6.7   5.6   4.7   4.7   4.2   3.9   51V   1.4   1.2   1.0   1.0   0.9   0.8   53Cr   4.1   3.4   2.9   2.8   2.6   2.4   55Mn   8.9   7.5   6.3   6.2   5.7   5.2   57Fe   4.3   3.6   3.0   3.0   2.8   2.5   59Co   11.4   9.5   8.0   7.9   7.2   6.6   61Ni   4.4   3.7   3.1   3.1   2.8   2.6   63Cu   6.0   5.0   4.2   4.2   3.8   3.5   65Cu   5.5   4.6   3.9   3.9   3.5   3.2   67Zn   4.1   3.4   2.9   2.8   3.5   2.4  

a  Mean  absolute  NQCC  errors  for  each  nuclide,  calculated  according  to  Eq.  49,  using  the  mean  absolute  error  of  Vzz  

from  Table  6  as  Vzz  value  and  Q  for  each  nuclide  is  taken  from  the  latest  set  of  quadrupole  moments  from  

Pyykkö.144  

   

Documento similar