2VAQ

STRUCTURE OF STRICTOSIDINE SYNTHASE IN COMPLEX WITH INHIBITOR


Experimental Data Snapshot

  • Method: X-RAY DIFFRACTION
  • Resolution: 3.01 Å
  • R-Value Free: 0.247 
  • R-Value Work: 0.186 
  • R-Value Observed: 0.189 

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This is version 1.4 of the entry. See complete history


Literature

Strictosidine synthase: mechanism of a Pictet-Spengler catalyzing enzyme.

Maresh, J.J.Giddings, L.A.Friedrich, A.Loris, E.A.Panjikar, S.Trout, B.L.Stockigt, J.Peters, B.O'Connor, S.E.

(2008) J Am Chem Soc 130: 710-723

  • DOI: https://doi.org/10.1021/ja077190z
  • Primary Citation of Related Structures:  
    2VAQ

  • PubMed Abstract: 

    The Pictet-Spengler reaction, which yields either a beta-carboline or a tetrahydroquinoline product from an aromatic amine and an aldehyde, is widely utilized in plant alkaloid biosynthesis. Here we deconvolute the role that the biosynthetic enzyme strictosidine synthase plays in catalyzing the stereoselective synthesis of a beta-carboline product. Notably, the rate-controlling step of the enzyme mechanism, as identified by the appearance of a primary kinetic isotope effect (KIE), is the rearomatization of a positively charged intermediate. The KIE of a nonenzymatic Pictet-Spengler reaction indicates that rearomatization is also rate-controlling in solution, suggesting that the enzyme does not significantly change the mechanism of the reaction. Additionally, the pH dependence of the solution and enzymatic reactions provides evidence for a sequence of acid-base catalysis steps that catalyze the Pictet-Spengler reaction. An additional acid-catalyzed step, most likely protonation of a carbinolamine intermediate, is also significantly rate controlling. We propose that this step is efficiently catalyzed by the enzyme. Structural analysis of a bisubstrate inhibitor bound to the enzyme suggests that the active site is exquisitely tuned to correctly orient the iminium intermediate for productive cyclization to form the diastereoselective product. Furthermore, ab initio calculations suggest the structures of possible productive transition states involved in the mechanism. Importantly, these calculations suggest that a spiroindolenine intermediate, often invoked in the Pictet-Spengler mechanism, does not occur. A detailed mechanism for enzymatic catalysis of the beta-carboline product is proposed from these data.


  • Organizational Affiliation

    Department of Chemistry, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139, USA.


Macromolecules
Find similar proteins by:  (by identity cutoff)  |  3D Structure
Entity ID: 1
MoleculeChains Sequence LengthOrganismDetailsImage
STRICTOSIDINE SYNTHASE
A, B
322Rauvolfia serpentinaMutation(s): 0 
EC: 4.3.3.2
UniProt
Find proteins for P68175 (Rauvolfia serpentina)
Explore P68175 
Go to UniProtKB:  P68175
Entity Groups  
Sequence Clusters30% Identity50% Identity70% Identity90% Identity95% Identity100% Identity
UniProt GroupP68175
Sequence Annotations
Expand
  • Reference Sequence
Small Molecules
Ligands 1 Unique
IDChains Name / Formula / InChI Key2D Diagram3D Interactions
VAW
Query on VAW

Download Ideal Coordinates CCD File 
C [auth A],
D [auth B]
(2S,3R,4S)-methyl 4-(2-(2-(1H-indol-3-yl)ethylamino)ethyl)-2-((2S,3R,4S,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)tetrahydro-2H-pyran-2-yloxy)-3-vinyl-3,4-dihydro-2H-pyran-5-carboxylate
C27 H36 N2 O9
MYFRJCYMRYXZQB-JVARDMDOSA-N
Binding Affinity Annotations 
IDSourceBinding Affinity
VAW PDBBind:  2VAQ IC50: 3 (nM) from 1 assay(s)
Experimental Data & Validation

Experimental Data

  • Method: X-RAY DIFFRACTION
  • Resolution: 3.01 Å
  • R-Value Free: 0.247 
  • R-Value Work: 0.186 
  • R-Value Observed: 0.189 
  • Space Group: H 3
Unit Cell:
Length ( Å )Angle ( ˚ )
a = 149.993α = 90
b = 149.993β = 90
c = 121.688γ = 120
Software Package:
Software NamePurpose
REFMACrefinement
DENZOdata reduction
SCALEPACKdata scaling
MOLREPphasing

Structure Validation

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Ligand Structure Quality Assessment 


Entry History 

Deposition Data

Revision History  (Full details and data files)

  • Version 1.0: 2008-09-16
    Type: Initial release
  • Version 1.1: 2011-07-13
    Changes: Advisory, Version format compliance
  • Version 1.2: 2018-02-07
    Changes: Database references, Source and taxonomy, Structure summary
  • Version 1.3: 2019-07-24
    Changes: Data collection
  • Version 1.4: 2023-12-13
    Changes: Data collection, Database references, Other, Refinement description