data_15629 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Conformation A configuration delta 7 and 8 and Conformation B Configuration lambda 4 of the Metal-Bound Pyoverdine PvdI, a siderophore of Pseudomonas aeruginosa ; _BMRB_accession_number 15629 _BMRB_flat_file_name bmr15629.str _Entry_type original _Submission_date 2008-01-21 _Accession_date 2008-01-21 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details ; The studied system is pyoverdine Pvd1-Ga(III) complex (studied at 253K). This system is obviously showing two different sets of chemical shifts. The result is the achievement of two distinct conformers: Pvd1_A and Pvd1_B, which have distinct chemical shifts sets and distinct restraints. The metal ion coordination site of each of these conformers can have 16 distinct geometric configurations: eight delta (D) configurations (noticed from 1D to 8D) and eight lambda (L) configurations (noticed from 1L to 8L). Because of a lack of obvious experimental data to define the geometry of this metal ion coordination site we defined them with imposed distances and distinct sets of improper angles, one for each geometry (based on previously published siderophore-metal ion complex structures). As a result of the computations we got one geometry for the B conformer (PvdI-Ga(III) B geometry 4L) but two geometries fo the A conformer (PvdI-Ga(III) A geometry 7D and PvdI-Ga(III) A geometry 8D). ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Wasielewski Emeric . . 2 Tzou Der-Lii . . 3 Dillmann Baudouin . . 4 Czaplicki Jerzy . . 5 Abdallah Mohamed A. . 6 Atkinson Andrew R. . 7 Kieffer Bruno . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 coupling_constants 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 134 "13C chemical shifts" 82 "15N chemical shifts" 20 "coupling constants" 11 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2008-06-27 original author . stop_ _Original_release_date 2008-06-27 save_ ############################# # Citation for this entry # ############################# save_citation_2 _Saveframe_category entry_citation _Citation_full . _Citation_title 'Multiple conformations of the metal-bound pyoverdine PvdI, a siderophore of Pseudomonas aeruginosa: a nuclear magnetic resonance study' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 18298082 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Wasielewski Emeric . . 2 Tzou Der-Lii . . 3 Dillmann Baudouin . . 4 Czaplicki Jerzy . . 5 Abdallah Mohamed A. . 6 Atkinson Andrew R. . 7 Kieffer Bruno . . stop_ _Journal_abbreviation Biochemistry _Journal_name_full Biochemistry _Journal_volume 47 _Journal_issue 11 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 3397 _Page_last 3406 _Year 2008 _Details . loop_ _Keyword 'conformational exchange' 'iron transport' 'isotopic labelling' NMR siderophore stop_ save_ ####################################### # Cited references within the entry # ####################################### save_citation_1 _Saveframe_category citation _Citation_full . _Citation_title 'A Low-Temperature Heteronuclear NMR Study of Two Exchanging Conformation s of Metal-Bound Pyoverdin PaA from Pseudomonas aeruginosa' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 16078193 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Tzou Der-Lii . . 2 Wasielewski Emeric . . 3 Abdallah Mohamed A. . 4 Kieffer Bruno . . 5 Atkinson Andrew R. . stop_ _Journal_abbreviation Biopolymers _Journal_name_full Biopolymers _Journal_volume 79 _Journal_issue 3 _Journal_CSD . _Book_title . _Book_chapter_title . _Book_volume . _Book_series . _Book_publisher . _Book_publisher_city . _Book_ISBN . _Conference_title . _Conference_site . _Conference_state_province . _Conference_country . _Conference_start_date . _Conference_end_date . _Conference_abstract_number . _Thesis_institution . _Thesis_institution_city . _Thesis_institution_country . _Page_first 139 _Page_last 149 _Year 2005 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'complex pyoverdine PvdI-Ga(III)' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'Pvd1, conformer A' $Pvd1 'Pvd1, conformer B' $Pvd1 'GALLIUM (III) ION, A' $GA 'GALLIUM (III) ION, B' $GA stop_ _System_molecular_weight . _System_physical_state bound _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . loop_ _Biological_function 'iron carrier for Gram-negative bacterium Pseudomonas aeruginosa ATCC 15692' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Pvd1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Pvd1 _Molecular_mass 1572.727 _Mol_thiol_state 'all free' loop_ _Biological_function siderophore stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 9 _Mol_residue_sequence XSRSXKXTT loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 0 CHR 2 1 SER 3 2 ARG 4 3 SER 5 4 OHO 6 5 LYS 7 6 OHO 8 7 THR 9 8 THR stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_CHR _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common 2,3-DIAMINO-6,7-DIHYDROXYQUINOLINE-BASED-CHROMOPHORE _BMRB_code . _PDB_code CHR _Standard_residue_derivative . _Molecular_mass 659.636 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 19:43:34 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C1 C1 C N 0 . ? C10 C10 C R 0 . ? C11 C11 C R 0 . ? C12 C12 C N 0 . ? C13 C13 C R 0 . ? C14 C14 C R 0 . ? C15 C15 C R 0 . ? C16 C16 C R 0 . ? C17 C17 C R 0 . ? C18 C18 C N 0 . ? C19 C19 C N 0 . ? C2 C2 C N 0 . ? C20 C20 C N 0 . ? C21 C21 C N 0 . ? C22 C22 C N 0 . ? C23 C23 C N 0 . ? C24 C24 C N 0 . ? C25 C25 C N 0 . ? C26 C26 C N 0 . ? C27 C27 C N 0 . ? C28 C28 C N 0 . ? C29 C29 C N 0 . ? C3 C3 C N 0 . ? C30 C30 C N 0 . ? C31 C31 C N 0 . ? C32 C32 C N 0 . ? C33 C33 C R 0 . ? C34 C34 C N 0 . ? C35 C35 C N 0 . ? C4 C4 C S 0 . ? C5 C5 C R 0 . ? C6 C6 C N 0 . ? C7 C7 C N 0 . ? C8 C8 C N 0 . ? C9 C9 C N 0 . ? H10 H10 H N 0 . ? H11 H11 H N 0 . ? H12 H12 H N 0 . ? H13 H13 H N 0 . ? H14 H14 H N 0 . ? H15 H15 H N 0 . ? H16 H16 H N 0 . ? H17 H17 H N 0 . ? H181 H181 H N 0 . ? H182 H182 H N 0 . ? H183 H183 H N 0 . ? H191 H191 H N 0 . ? H192 H192 H N 0 . ? H193 H193 H N 0 . ? H23 H23 H N 0 . ? H24 H24 H N 0 . ? H27 H27 H N 0 . ? H29 H29 H N 0 . ? H311 H311 H N 0 . ? H312 H312 H N 0 . ? H313 H313 H N 0 . ? H321 H321 H N 0 . ? H322 H322 H N 0 . ? H323 H323 H N 0 . ? H33 H33 H N 0 . ? H351 H351 H N 0 . ? H352 H352 H N 0 . ? H5 H5 H N 0 . ? H8 H8 H N 0 . ? HN1 HN1 H N 0 . ? HO4 HO4 H N 0 . ? HO5 HO5 H N 0 . ? HO9 HO9 H N 0 . ? N1 N1 N N 0 . ? O1 O1 O N 0 . ? O10 O10 O N 0 . ? O11 O11 O N 0 . ? O12 O12 O N 0 . ? O2 O2 O N 0 . ? O3 O3 O N 0 . ? O4 O4 O N 0 . ? O5 O5 O N 0 . ? O6 O6 O N 0 . ? O7 O7 O N 0 . ? O8 O8 O N 0 . ? O9 O9 O N 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING C1 C2 ? ? SING C1 C9 ? ? DOUB C1 C12 ? ? TRIP C2 C3 ? ? SING C3 C4 ? ? SING C4 O2 ? ? SING C4 C5 ? ? SING C4 C33 ? ? SING O2 C5 ? ? SING C5 C6 ? ? SING C5 H5 ? ? TRIP C6 C7 ? ? SING C7 C8 ? ? DOUB C8 C9 ? ? SING C8 H8 ? ? SING C9 C10 ? ? SING C10 O1 ? ? SING C10 C11 ? ? SING C10 H10 ? ? SING O1 C13 ? ? SING C11 O6 ? ? SING C11 C12 ? ? SING C11 H11 ? ? SING O6 C20 ? ? SING C12 H12 ? ? SING C13 O3 ? ? SING C13 C14 ? ? SING C13 H13 ? ? SING O3 C17 ? ? SING C14 N1 ? ? SING C14 C15 ? ? SING C14 H14 ? ? SING N1 C19 ? ? SING N1 HN1 ? ? SING C19 H191 ? ? SING C19 H192 ? ? SING C19 H193 ? ? SING C15 O4 ? ? SING C15 C16 ? ? SING C15 H15 ? ? SING O4 HO4 ? ? SING C16 O5 ? ? SING C16 C17 ? ? SING C16 H16 ? ? SING O5 HO5 ? ? SING C17 C18 ? ? SING C17 H17 ? ? SING C18 H181 ? ? SING C18 H182 ? ? SING C18 H183 ? ? DOUB C20 O7 ? ? SING C20 C21 ? ? DOUB C21 C22 ? ? SING C21 C26 ? ? SING C22 O9 ? ? SING C22 C23 ? ? SING O9 HO9 ? ? DOUB C23 C24 ? ? SING C23 H23 ? ? SING C24 C25 ? ? SING C24 H24 ? ? DOUB C25 C26 ? ? SING C25 C30 ? ? SING C26 C27 ? ? DOUB C27 C28 ? ? SING C27 H27 ? ? SING C28 O8 ? ? SING C28 C29 ? ? SING O8 C31 ? ? SING C31 H311 ? ? SING C31 H312 ? ? SING C31 H313 ? ? DOUB C29 C30 ? ? SING C29 H29 ? ? SING C30 C32 ? ? SING C32 H321 ? ? SING C32 H322 ? ? SING C32 H323 ? ? SING C33 O10 ? ? SING C33 C35 ? ? SING C33 H33 ? ? SING O10 C34 ? ? DOUB C34 O11 ? ? SING C34 O12 ? ? SING O12 C35 ? ? SING C35 H351 ? ? SING C35 H352 ? ? stop_ save_ save_chem_comp_OHO _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common N-FORMYL-N-HYDROXYORNITHINE _BMRB_code . _PDB_code OHO _Standard_residue_derivative . _Molecular_mass 143.184 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Tue Aug 21 00:45:57 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C N 0 . ? C1 C1 C N 0 . ? C2 C2 C N 0 . ? C3 C3 C N 0 . ? C4 C4 C N 0 . ? C5 C5 C N 0 . ? C6 C6 C N 0 . ? H1 H1 H N 0 . ? H21 H21 H N 0 . ? H22 H22 H N 0 . ? H31 H31 H N 0 . ? H32 H32 H N 0 . ? H41 H41 H N 0 . ? H42 H42 H N 0 . ? H51 H51 H N 0 . ? H52 H52 H N 0 . ? H61 H61 H N 0 . ? H62 H62 H N 0 . ? HN HN H N 0 . ? HXT HXT H N 0 . ? N N N N 0 . ? O O O N 0 . ? OXT OXT O N 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N C ? ? SING N C1 ? ? SING N HN ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? SING C1 C2 ? ? SING C1 C6 ? ? SING C1 H1 ? ? SING C2 C3 ? ? SING C2 H21 ? ? SING C2 H22 ? ? SING C3 C4 ? ? SING C3 H31 ? ? SING C3 H32 ? ? SING C4 C5 ? ? SING C4 H41 ? ? SING C4 H42 ? ? SING C5 C6 ? ? SING C5 H51 ? ? SING C5 H52 ? ? SING C6 H61 ? ? SING C6 H62 ? ? stop_ save_ ############# # Ligands # ############# save_GA _Saveframe_category ligand _Mol_type non-polymer _Name_common "GA (GALLIUM (III) ION)" _BMRB_code . _PDB_code GA _Molecular_mass 69.723 _Mol_charge 3 _Mol_paramagnetic . _Mol_aromatic no _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 21:42:30 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons GA GA GA N 3 . ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Strain $Pvd1 'Pseudomonas aeruginosa' 287 Bacteria . Pseudomonas aeruginosa PAO2 stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $Pvd1 'purified from the natural source' . . . PAO2 . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_15N_labelled_sample _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 7 mM [U-15N] stop_ save_ save_13C_15N_labelled_sample _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 7 mM '[U-100% 13C; U-100% 15N]' stop_ save_ save_non_labelled_sample _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 7 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_X-PLOR_NIH _Saveframe_category software _Name 'X-PLOR NIH' _Version . loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task refinement 'structure solution' stop_ _Details . save_ save_XEASY _Saveframe_category software _Name XEASY _Version . loop_ _Vendor _Address _Electronic_address 'Bartels et al.' . . stop_ loop_ _Task 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_xwinnmr _Saveframe_category software _Name xwinnmr _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection stop_ _Details . save_ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details . save_ save_Molmol _Saveframe_category software _Name Molmol _Version . loop_ _Vendor _Address _Electronic_address 'Koradi, Billeter and Wuthrich' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_Felix _Saveframe_category software _Name FELIX _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Accelrys Software Inc.' . . stop_ loop_ _Task 'data analysis' processing stop_ _Details . save_ save_MATLAB _Saveframe_category software _Name MATLAB _Version . loop_ _Vendor _Address _Electronic_address 'The MathWorks Inc.' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $15N_labelled_sample save_ save_2D_1H-13C_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $13C_15N_labelled_sample save_ save_Off-resonance_ROESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name 'Off-resonance ROESY' _Sample_label $non_labelled_sample save_ save_3D_HNCA_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $13C_15N_labelled_sample save_ save_3D_CBCA(CO)NH_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCA(CO)NH' _Sample_label $13C_15N_labelled_sample save_ save_3D_HNCACB_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACB' _Sample_label $13C_15N_labelled_sample save_ save_3D_HNCO_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $13C_15N_labelled_sample save_ save_3D_HN(CO)CA_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HN(CO)CA' _Sample_label $13C_15N_labelled_sample save_ save_3D_HCCH-COSY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY' _Sample_label $13C_15N_labelled_sample save_ save_3D_HCCH-TOCSY_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _Sample_label $13C_15N_labelled_sample save_ save_3D_HCCH-COSY_11 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY' _Sample_label $13C_15N_labelled_sample save_ save_3D_HCCH-TOCSY_12 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _Sample_label $13C_15N_labelled_sample save_ save_2D_1H-1H_NOESY_13 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $non_labelled_sample save_ save_2D_1H-1H_NOESY_14 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $non_labelled_sample save_ save_2D_1H-15N_CT-HMQC-J_15 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N CT-HMQC-J' _Sample_label $15N_labelled_sample save_ save_2D_1H-15N_CT-HMQC-J_16 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N CT-HMQC-J' _Sample_label $15N_labelled_sample save_ save_2D_1H-1H_TOCSY_17 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $non_labelled_sample save_ save_2D_1H-1H_TOCSY_18 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $non_labelled_sample save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.6 . pH pressure 1 . atm temperature 253 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.6 . pH pressure 1 . atm temperature 267 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS C 13 'methyl protons' ppm 0.00 . indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 . indirect . . . 0.101329118 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details 'For conformer A PvdI-Ga(III): two geometries 7D and 8D.' loop_ _Software_label $XEASY stop_ loop_ _Experiment_label '2D 1H-15N HSQC' 'Off-resonance ROESY' '3D HNCO' '3D HCCH-COSY' '3D HCCH-TOCSY' '2D 1H-1H NOESY' '2D 1H-1H TOCSY' stop_ loop_ _Sample_label $15N_labelled_sample $non_labelled_sample $13C_15N_labelled_sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'Pvd1, conformer B' _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 0 1 CHR H H 9.72 0.02 1 2 0 1 CHR HA H 2.81 0.02 2 3 0 1 CHR HB H 2.81 0.02 2 4 0 1 CHR CA C 31.40 0.25 1 5 0 1 CHR CB C 30.30 0.25 1 6 0 1 CHR C C 179.30 0.25 1 7 0 1 CHR N N 117.95 0.10 1 8 0 1 CHR H4 H 6.70 0.02 1 9 0 1 CHR H5 H 7.72 0.02 1 10 0 1 CHR H8 H 6.99 0.02 1 11 0 1 CHR H11 H 5.83 0.02 1 12 0 1 CHR H121 H 2.63 0.02 1 13 0 1 CHR H122 H 2.43 0.02 1 14 0 1 CHR H131 H 3.68 0.02 1 15 0 1 CHR H132 H 3.44 0.02 1 16 0 1 CHR C11 C 57.40 0.25 1 17 0 1 CHR C12 C 23.10 0.25 1 18 0 1 CHR C13 C 36.20 0.25 1 19 1 2 SER H H 9.91 0.02 1 20 1 2 SER HA H 4.22 0.02 1 21 1 2 SER HB2 H 4.06 0.02 2 22 1 2 SER HB3 H 4.06 0.02 2 23 1 2 SER CA C 60.20 0.25 1 24 1 2 SER CB C 61.90 0.25 1 25 1 2 SER C C 175.70 0.25 1 26 1 2 SER N N 118.61 0.10 1 27 2 3 ARG H H 8.18 0.02 1 28 2 3 ARG HA H 4.26 0.02 1 29 2 3 ARG HB2 H 1.81 0.02 2 30 2 3 ARG HB3 H 1.81 0.02 2 31 2 3 ARG HG2 H 0.92 0.02 2 32 2 3 ARG HG3 H 0.66 0.02 2 33 2 3 ARG HD2 H 2.58 0.02 2 34 2 3 ARG HD3 H 2.19 0.02 2 35 2 3 ARG HE H 6.55 0.02 1 36 2 3 ARG CA C 55.70 0.25 1 37 2 3 ARG CB C 29.80 0.25 1 38 2 3 ARG CG C 26.50 0.25 1 39 2 3 ARG CD C 41.70 0.25 1 40 2 3 ARG CZ C 180.80 0.25 1 41 2 3 ARG C C 177.60 0.25 1 42 2 3 ARG N N 117.63 0.10 1 43 2 3 ARG NE N 83.93 0.10 1 44 3 4 SER H H 8.12 0.02 1 45 3 4 SER HA H 4.05 0.02 1 46 3 4 SER HB2 H 3.91 0.02 2 47 3 4 SER HB3 H 3.91 0.02 2 48 3 4 SER CA C 59.60 0.25 1 49 3 4 SER CB C 61.50 0.25 1 50 3 4 SER C C 175.20 0.25 1 51 3 4 SER N N 114.04 0.10 1 52 4 5 OHO H H 7.61 0.02 1 53 4 5 OHO HA H 4.30 0.02 1 54 4 5 OHO HB2 H 1.77 0.02 2 55 4 5 OHO HB3 H 1.77 0.02 2 56 4 5 OHO HG2 H 2.00 0.02 1 57 4 5 OHO HG3 H 1.42 0.02 1 58 4 5 OHO HD2 H 3.68 0.02 1 59 4 5 OHO HD3 H 3.62 0.02 1 60 4 5 OHO HZ H 7.90 0.02 1 61 4 5 OHO CA C 55.20 0.25 1 62 4 5 OHO CB C 28.20 0.25 1 63 4 5 OHO CG C 23.80 0.25 1 64 4 5 OHO CD C 51.30 0.25 1 65 4 5 OHO C C 177.40 0.25 1 66 4 5 OHO N N 117.64 0.10 1 67 5 6 LYS H H 8.73 0.02 1 68 5 6 LYS HA H 4.09 0.02 1 69 5 6 LYS HB2 H 1.89 0.02 2 70 5 6 LYS HB3 H 1.81 0.02 2 71 5 6 LYS HG2 H 1.30 0.02 2 72 5 6 LYS HG3 H 1.30 0.02 2 73 5 6 LYS HD2 H 1.65 0.02 2 74 5 6 LYS HD3 H 1.59 0.02 2 75 5 6 LYS HE2 H 3.48 0.02 2 76 5 6 LYS HE3 H 3.03 0.02 2 77 5 6 LYS HZ H 7.59 0.02 1 78 5 6 LYS CA C 55.90 0.25 1 79 5 6 LYS CB C 31.10 0.25 1 80 5 6 LYS CG C 23.30 0.25 1 81 5 6 LYS CD C 28.20 0.25 1 82 5 6 LYS CE C 40.60 0.25 1 83 5 6 LYS N N 123.26 0.10 1 84 5 6 LYS NZ N 118.45 0.10 1 85 6 7 OHO H H 8.61 0.02 1 86 6 7 OHO HA H 4.29 0.02 1 87 6 7 OHO HB2 H 1.92 0.02 2 88 6 7 OHO HB3 H 1.92 0.02 2 89 6 7 OHO HG2 H 1.40 0.02 2 90 6 7 OHO HG3 H 1.40 0.02 2 91 6 7 OHO HD2 H 3.67 0.02 1 92 6 7 OHO HD3 H 3.62 0.02 1 93 6 7 OHO HZ H 7.88 0.02 1 94 6 7 OHO CA C 55.30 0.25 1 95 6 7 OHO CB C 28.20 0.25 1 96 6 7 OHO CG C 26.10 0.25 1 97 6 7 OHO CD C 52.30 0.25 1 98 6 7 OHO C C 177.50 0.25 1 99 7 8 THR H H 7.75 0.02 1 100 7 8 THR HA H 4.40 0.02 1 101 7 8 THR HB H 4.55 0.02 1 102 7 8 THR HG1 H 6.17 0.02 1 103 7 8 THR HG2 H 1.30 0.02 2 104 7 8 THR CA C 61.30 0.25 1 105 7 8 THR CB C 67.80 0.25 1 106 7 8 THR CG2 C 20.80 0.25 1 107 7 8 THR C C 175.20 0.25 1 108 7 8 THR N N 109.73 0.10 1 109 8 9 THR H H 7.87 0.02 1 110 8 9 THR HA H 4.36 0.02 1 111 8 9 THR HB H 4.46 0.02 1 112 8 9 THR HG1 H 5.85 0.02 1 113 8 9 THR HG2 H 1.25 0.02 2 114 8 9 THR CA C 60.10 0.25 1 115 8 9 THR CB C 67.50 0.25 1 116 8 9 THR CG2 C 20.60 0.25 1 117 8 9 THR C C 174.70 0.25 1 118 8 9 THR N N 110.59 0.10 1 stop_ save_ save_assigned_chem_shift_list_2 _Saveframe_category assigned_chemical_shifts _Details 'For conformer B PvdI-Ga(III).' loop_ _Software_label $XEASY stop_ loop_ _Experiment_label '2D 1H-15N HSQC' 'Off-resonance ROESY' '3D HNCO' '3D HCCH-COSY' '3D HCCH-TOCSY' '2D 1H-1H NOESY' '2D 1H-1H TOCSY' stop_ loop_ _Sample_label $15N_labelled_sample $non_labelled_sample $13C_15N_labelled_sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'Pvd1, conformer B' _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 0 1 CHR H H 9.72 0.02 . 2 0 1 CHR HA H 2.81 0.02 . 3 0 1 CHR HB H 2.81 0.02 . 4 0 1 CHR CA C 31.40 0.25 . 5 0 1 CHR CB C 30.30 0.25 . 6 0 1 CHR C C 179.30 0.25 . 7 0 1 CHR N N 117.95 0.10 . 8 0 1 CHR H4 H 6.70 0.02 . 9 0 1 CHR H5 H 7.72 0.02 . 10 0 1 CHR H8 H 6.99 0.02 . 11 0 1 CHR H11 H 5.83 0.02 . 12 0 1 CHR H121 H 2.63 0.02 . 13 0 1 CHR H122 H 2.43 0.02 . 14 0 1 CHR H131 H 3.68 0.02 . 15 0 1 CHR H132 H 3.44 0.02 . 16 0 1 CHR C11 C 57.40 0.25 . 17 0 1 CHR C12 C 23.10 0.25 . 18 0 1 CHR C13 C 36.20 0.25 . 19 1 2 SER H H 9.91 0.02 1 20 1 2 SER HA H 4.22 0.02 1 21 1 2 SER HB2 H 4.06 0.02 2 22 1 2 SER HB3 H 4.06 0.02 2 23 1 2 SER CA C 60.20 0.25 1 24 1 2 SER CB C 61.90 0.25 1 25 1 2 SER C C 175.70 0.25 1 26 1 2 SER N N 118.61 0.10 1 27 2 3 ARG H H 8.18 0.02 1 28 2 3 ARG HA H 4.26 0.02 1 29 2 3 ARG HB2 H 1.81 0.02 2 30 2 3 ARG HB3 H 1.81 0.02 2 31 2 3 ARG HG2 H 0.92 0.02 2 32 2 3 ARG HG3 H 0.66 0.02 2 33 2 3 ARG HD2 H 2.58 0.02 2 34 2 3 ARG HD3 H 2.19 0.02 2 35 2 3 ARG HE H 6.55 0.02 1 36 2 3 ARG CA C 55.70 0.25 1 37 2 3 ARG CB C 29.80 0.25 1 38 2 3 ARG CG C 26.50 0.25 1 39 2 3 ARG CD C 41.70 0.25 1 40 2 3 ARG CZ C 180.80 0.25 1 41 2 3 ARG C C 177.60 0.25 1 42 2 3 ARG N N 117.63 0.10 1 43 2 3 ARG NE N 83.93 0.10 1 44 3 4 SER H H 8.12 0.02 1 45 3 4 SER HA H 4.05 0.02 1 46 3 4 SER HB2 H 3.91 0.02 2 47 3 4 SER HB3 H 3.91 0.02 2 48 3 4 SER CA C 59.60 0.25 1 49 3 4 SER CB C 61.50 0.25 1 50 3 4 SER C C 175.20 0.25 1 51 3 4 SER N N 114.04 0.10 1 52 4 5 OHO H H 7.61 0.02 . 53 4 5 OHO HA H 4.30 0.02 . 54 4 5 OHO HB2 H 1.77 0.02 . 55 4 5 OHO HB3 H 1.77 0.02 . 56 4 5 OHO HG2 H 2.00 0.02 . 57 4 5 OHO HG3 H 1.42 0.02 . 58 4 5 OHO HD2 H 3.68 0.02 . 59 4 5 OHO HD3 H 3.62 0.02 . 60 4 5 OHO HZ H 7.90 0.02 . 61 4 5 OHO CA C 55.20 0.25 . 62 4 5 OHO CB C 28.20 0.25 . 63 4 5 OHO CG C 23.80 0.25 . 64 4 5 OHO CD C 51.30 0.25 . 65 4 5 OHO C C 177.40 0.25 . 66 4 5 OHO N N 117.64 0.10 . 67 5 6 LYS H H 8.73 0.02 1 68 5 6 LYS HA H 4.09 0.02 1 69 5 6 LYS HB2 H 1.89 0.02 2 70 5 6 LYS HB3 H 1.81 0.02 2 71 5 6 LYS HG2 H 1.30 0.02 2 72 5 6 LYS HG3 H 1.30 0.02 2 73 5 6 LYS HD2 H 1.65 0.02 2 74 5 6 LYS HD3 H 1.59 0.02 2 75 5 6 LYS HE2 H 3.48 0.02 2 76 5 6 LYS HE3 H 3.03 0.02 2 77 5 6 LYS HZ H 7.59 0.02 1 78 5 6 LYS CA C 55.90 0.25 1 79 5 6 LYS CB C 31.10 0.25 1 80 5 6 LYS CG C 23.30 0.25 1 81 5 6 LYS CD C 28.20 0.25 1 82 5 6 LYS CE C 40.60 0.25 1 83 5 6 LYS N N 123.26 0.10 1 84 5 6 LYS NZ N 118.45 0.10 1 85 6 7 OHO H H 8.61 0.02 . 86 6 7 OHO HA H 4.29 0.02 . 87 6 7 OHO HB2 H 1.92 0.02 . 88 6 7 OHO HB3 H 1.92 0.02 . 89 6 7 OHO HG2 H 1.40 0.02 . 90 6 7 OHO HG3 H 1.40 0.02 . 91 6 7 OHO HD2 H 3.67 0.02 . 92 6 7 OHO HD3 H 3.62 0.02 . 93 6 7 OHO HZ H 7.88 0.02 . 94 6 7 OHO CA C 55.30 0.25 . 95 6 7 OHO CB C 28.20 0.25 . 96 6 7 OHO CG C 26.10 0.25 . 97 6 7 OHO CD C 52.30 0.25 . 98 6 7 OHO C C 177.50 0.25 . 99 7 8 THR H H 7.75 0.02 1 100 7 8 THR HA H 4.40 0.02 1 101 7 8 THR HB H 4.55 0.02 1 102 7 8 THR HG1 H 6.17 0.02 1 103 7 8 THR HG2 H 1.30 0.02 . 104 7 8 THR CA C 61.30 0.25 1 105 7 8 THR CB C 67.80 0.25 1 106 7 8 THR CG2 C 20.80 0.25 1 107 7 8 THR C C 175.20 0.25 1 108 7 8 THR N N 109.73 0.10 1 109 8 9 THR H H 7.87 0.02 1 110 8 9 THR HA H 4.36 0.02 1 111 8 9 THR HB H 4.46 0.02 1 112 8 9 THR HG1 H 5.85 0.02 1 113 8 9 THR HG2 H 1.25 0.02 . 114 8 9 THR CA C 60.10 0.25 1 115 8 9 THR CB C 67.50 0.25 1 116 8 9 THR CG2 C 20.60 0.25 1 117 8 9 THR C C 174.70 0.25 1 118 8 9 THR N N 110.59 0.10 1 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants _Details 'For conformer A PvdI-Ga(III): two geometries 7D and 8D.' loop_ _Software_label $MATLAB stop_ loop_ _Experiment_label '2D 1H-15N CT-HMQC-J' stop_ _Sample_conditions_label $sample_conditions_2 _Spectrometer_frequency_1H 600 _Mol_system_component_name 'Pvd1, conformer A' _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 2 SER H 2 SER HA 3.88 . . 2.1 2 3JHNHA 3 ARG H 3 ARG HA 9.34 . . 0.1 3 3JHNHA 4 SER H 4 SER HA 5.87 . . 0.1 4 3JHNHA 7 OHO H 7 OHO HA 6.16 . . 3.7 5 3JHNHA 8 THR H 8 THR HA 8.43 . . 2.9 6 3JHNHA 9 THR H 9 THR HA 7.35 . . 0.1 stop_ save_ save_coupling_constant_list_2 _Saveframe_category coupling_constants _Details 'For conformer B PvdI-Ga(III).' loop_ _Software_label $MATLAB stop_ loop_ _Experiment_label '2D 1H-15N CT-HMQC-J' stop_ _Sample_conditions_label $sample_conditions_2 _Spectrometer_frequency_1H 600 _Mol_system_component_name 'Pvd1, conformer B' _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 2 SER H 2 SER HA 5.17 . . 2.5 2 3JHNHA 3 ARG H 3 ARG HA 8.69 . . 0.1 3 3JHNHA 4 SER H 4 SER HA 4.58 . . 0.1 4 3JHNHA 8 THR H 8 THR HA 7.94 . . 1.6 5 3JHNHA 9 THR H 9 THR HA 8.47 . . 3.3 stop_ save_