data_5112 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; High-resolution Structures for the Psi-conotoxins Indicate Differences in Disulfide Bridge Dynamics ; _BMRB_accession_number 5112 _BMRB_flat_file_name bmr5112.str _Entry_type original _Submission_date 2001-08-15 _Accession_date 2001-08-15 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 'Van Wagoner' R. M. . 2 Ireland C. M. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 138 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2008-08-07 update BMRB 'Updating non-standard residue' stop_ loop_ _Related_BMRB_accession_number _Relationship 5113 'psi-conotoxin PIIIE' stop_ _Original_release_date 2001-08-15 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; An Improved Solution Structure for Psi-conotoxin Piiie ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code 22651999 _PubMed_ID 12767215 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 'Van Wagoner' R. M. . 2 Ireland C. M. . stop_ _Journal_abbreviation Biochemistry _Journal_volume 42 _Journal_issue 21 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 6347 _Page_last 6352 _Year 2003 _Details . loop_ _Keyword 'amidated C-terminus' 'multiple disulfide bonds' stop_ save_ ################################## # Molecular system description # ################################## save_system_psi-conotoxin _Saveframe_category molecular_system _Mol_system_name 'PSI-CONOTOXIN PIIIF' _Abbreviation_common psi-conotoxin _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'psi-conotoxin PIIIF' $psi-conotoxin stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'all disulfide bound' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_psi-conotoxin _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common psi-conotoxin _Abbreviation_common psi-conotoxin _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 25 _Mol_residue_sequence ; GXXCCLYGSCRXFXGCYNAL CCRKX ; loop_ _Residue_seq_code _Residue_label 1 GLY 2 HYP 3 HYP 4 CYS 5 CYS 6 LEU 7 TYR 8 GLY 9 SER 10 CYS 11 ARG 12 HYP 13 PHE 14 HYP 15 GLY 16 CYS 17 TYR 18 ASN 19 ALA 20 LEU 21 CYS 22 CYS 23 ARG 24 LYS 25 NH2 stop_ _Sequence_homology_query_date 2008-03-24 _Sequence_homology_query_revised_last_date 2008-03-03 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value PDB 1JLP 'A Chain A, Solution Structure Of TheNoncompetitive Skeletal Muscle Nicotinic AcetylcholineReceptor Antagonist Psi-Conoto' 100.00 24 100 100 3e-05 stop_ save_ ###################### # Polymer residues # ###################### save_chem_comp_HYP _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 4-HYDROXYPROLINE _BMRB_code HYP _PDB_code HYP _Standard_residue_derivative . _Molecular_mass 131.130 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? OD1 OD1 O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG HG H . 0 . ? HD22 HD22 H . 0 . ? HD23 HD23 H . 0 . ? HD1 HD1 H . 0 . ? HXT HXT H . 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 CA ? ? SING N CD ? ? SING N H ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG OD1 ? ? SING CG HG ? ? SING CD HD22 ? ? SING CD HD23 ? ? SING OD1 HD1 ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common 'AMINO GROUP' _BMRB_code . _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Thu Jul 21 10:41:13 2011 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 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 HN1 ? ? SING N HN2 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $psi-conotoxin 'purple cone' 41690 Eukaryota Metazoa Conus purpurascens 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 $psi-conotoxin 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $psi-conotoxin 12 mM . 'tetra-TFA salt' 12 mM . H2O 90 % . D2O 10 % . stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $psi-conotoxin 12 mM . 'tetra-TFA salt' 12 mM . D2O 100 % . stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details 'The cysteine used was 13C-labeled only at position 3 (i.e. the beta carbon).' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $psi-conotoxin 14 mM [U-13CB]-Cys5,Cys10,Cys16,Cys21,Cys22 'tetra-TFA salt' 12 mM . H2O 90 % . D2O 10 % . stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type solution _Details 'The cysteine used was 13C-labeled only at position 3 (i.e. the beta carbon).' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $psi-conotoxin 16 mM [U-13CB]-Cys4 'tetra-TFA salt' 12 mM . H2O 90 % . D2O 10 % . stop_ save_ save_sample_5 _Saveframe_category sample _Sample_type solution _Details 'The cysteine used was 13C-labeled only at position 3 (i.e. the beta carbon).' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $psi-conotoxin 16 mM [U-13CB]-Cys4 'tetra-TFA salt' 12 mM . D2O 100 % . stop_ save_ ############################ # Computer software used # ############################ save_VNMR _Saveframe_category software _Name VNMR _Version 6.1B loop_ _Task collection stop_ _Details 'Varian, Inc.' save_ save_FELIX _Saveframe_category software _Name FELIX _Version 97.0 loop_ _Task processing stop_ _Details 'MSI, Inc.' save_ save_IRMA _Saveframe_category software _Name IRMA _Version 97.0 loop_ _Task 'iterative matrix relaxation' stop_ _Details 'MSI, Inc.' save_ save_DGII _Saveframe_category software _Name DGII _Version 97.0 loop_ _Task 'structure solution' stop_ _Details 'MSI, Inc.' save_ save_DISCOVER _Saveframe_category software _Name DISCOVER _Version 2.98 loop_ _Task 'structure solution' stop_ _Details 'MSI, Inc.' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NOESY' _Sample_label . save_ save_DQF-COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name DQF-COSY _Sample_label . save_ save_PE-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name PE-COSY _Sample_label . save_ save_13C-selected_2D_NOESY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '13C-selected 2D NOESY' _Sample_label . save_ save_Double_half-filtered_2D_NOESY_5 _Saveframe_category NMR_applied_experiment _Experiment_name 'Double half-filtered 2D NOESY' _Sample_label . save_ save_Double_half-filtered_2D_PE-COSY_6 _Saveframe_category NMR_applied_experiment _Experiment_name 'Double half-filtered 2D PE-COSY' _Sample_label . save_ save_13C-selected_1D_1H_NMR_7 _Saveframe_category NMR_applied_experiment _Experiment_name '13C-selected 1D 1H NMR' _Sample_label . save_ ####################### # Sample conditions # ####################### save_sample_cond_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 12 . mM pH 3.5 . n/a pressure 1 . atm temperature 277 . K stop_ save_ save_sample_cond_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 12 . mM pH 3.5 . n/a pressure 1 . atm temperature 295 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference _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 water H 1 protons ppm 4.93 . . . . . 1.0 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_chemical_shift_set_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_cond_1 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name 'psi-conotoxin PIIIF' _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 . 1 GLY H H 8.04 0.1 1 2 . 1 GLY HA2 H 3.94 0.1 2 3 . 1 GLY HA3 H 3.83 0.1 2 4 . 2 HYP HA H 4.73 0.1 1 5 . 2 HYP HB2 H 2.11 0.1 1 6 . 2 HYP HB3 H 1.51 0.1 1 7 . 2 HYP HG H 4.08 0.1 1 8 . 2 HYP HD22 H 3.39 0.1 2 9 . 2 HYP HD23 H 3.19 0.1 2 10 . 3 HYP HA H 4.62 0.1 1 11 . 3 HYP HB2 H 2.37 0.1 1 12 . 3 HYP HB3 H 2.04 0.1 1 13 . 3 HYP HG H 4.58 0.1 1 14 . 3 HYP HD22 H 3.83 0.1 2 15 . 3 HYP HD23 H 3.62 0.1 2 16 . 4 CYS H H 8.72 0.1 1 17 . 4 CYS HA H 4.75 0.1 1 18 . 4 CYS HB2 H 3.07 0.1 1 19 . 4 CYS HB3 H 2.85 0.1 1 20 . 5 CYS H H 7.94 0.1 1 21 . 5 CYS HA H 5.35 0.1 1 22 . 5 CYS HB2 H 2.82 0.1 1 23 . 5 CYS HB3 H 3.01 0.1 1 24 . 6 LEU H H 8.25 0.1 1 25 . 6 LEU HA H 4.26 0.1 1 26 . 6 LEU HB2 H 1.41 0.1 2 27 . 6 LEU HB3 H 1.17 0.1 2 28 . 6 LEU HG H 1.00 0.1 1 29 . 6 LEU HD1 H 0.77 0.1 2 30 . 6 LEU HD2 H 0.67 0.1 2 31 . 7 TYR H H 9.28 0.1 1 32 . 7 TYR HA H 4.34 0.1 1 33 . 7 TYR HB2 H 3.04 0.1 1 34 . 7 TYR HB3 H 3.28 0.1 1 35 . 7 TYR HD1 H 7.07 0.1 1 36 . 7 TYR HD2 H 7.07 0.1 1 37 . 7 TYR HE1 H 6.82 0.1 1 38 . 7 TYR HE2 H 6.82 0.1 1 39 . 8 GLY H H 8.63 0.1 1 40 . 8 GLY HA2 H 3.65 0.1 1 41 . 8 GLY HA3 H 4.23 0.1 1 42 . 9 SER H H 7.80 0.1 1 43 . 9 SER HA H 4.72 0.1 1 44 . 9 SER HB2 H 3.87 0.1 2 45 . 9 SER HB3 H 3.80 0.1 2 46 . 10 CYS H H 8.71 0.1 1 47 . 10 CYS HA H 4.74 0.1 1 48 . 10 CYS HB2 H 3.06 0.1 2 49 . 10 CYS HB3 H 2.97 0.1 2 50 . 11 ARG H H 8.81 0.1 1 51 . 11 ARG HA H 4.62 0.1 1 52 . 11 ARG HB2 H 1.46 0.1 1 53 . 11 ARG HB3 H 1.75 0.1 1 54 . 11 ARG HG2 H 1.59 0.1 1 55 . 11 ARG HG3 H 1.59 0.1 1 56 . 11 ARG HD2 H 3.14 0.1 1 57 . 11 ARG HD3 H 3.14 0.1 1 58 . 11 ARG HE H 7.00 0.1 1 59 . 12 HYP HA H 4.61 0.1 1 60 . 12 HYP HB2 H 1.93 0.1 1 61 . 12 HYP HB3 H 2.39 0.1 1 62 . 12 HYP HG H 4.38 0.1 1 63 . 12 HYP HD22 H 3.55 0.1 2 64 . 12 HYP HD23 H 3.55 0.1 2 65 . 13 PHE H H 7.86 0.1 1 66 . 13 PHE HA H 4.81 0.1 1 67 . 13 PHE HB2 H 2.88 0.1 1 68 . 13 PHE HB3 H 3.10 0.1 1 69 . 13 PHE HD1 H 7.23 0.1 1 70 . 13 PHE HD2 H 7.23 0.1 1 71 . 13 PHE HE1 H 7.30 0.1 1 72 . 13 PHE HE2 H 7.30 0.1 1 73 . 13 PHE HZ H 7.30 0.1 1 74 . 14 HYP HA H 4.56 0.1 1 75 . 14 HYP HB2 H 2.03 0.1 1 76 . 14 HYP HB3 H 2.32 0.1 1 77 . 14 HYP HG H 4.60 0.1 1 78 . 14 HYP HD22 H 3.84 0.1 1 79 . 14 HYP HD23 H 3.48 0.1 1 80 . 15 GLY H H 8.87 0.1 1 81 . 15 GLY HA2 H 3.84 0.1 1 82 . 15 GLY HA3 H 4.26 0.1 1 83 . 16 CYS H H 8.14 0.1 1 84 . 16 CYS HA H 4.95 0.1 1 85 . 16 CYS HB2 H 3.42 0.1 1 86 . 16 CYS HB3 H 3.08 0.1 1 87 . 17 TYR H H 7.89 0.1 1 88 . 17 TYR HA H 4.23 0.1 1 89 . 17 TYR HB2 H 3.07 0.1 2 90 . 17 TYR HB3 H 3.01 0.1 2 91 . 17 TYR HD1 H 7.10 0.1 1 92 . 17 TYR HD2 H 7.10 0.1 1 93 . 17 TYR HE1 H 6.81 0.1 1 94 . 17 TYR HE2 H 6.81 0.1 1 95 . 18 ASN H H 7.86 0.1 1 96 . 18 ASN HA H 4.66 0.1 1 97 . 18 ASN HB2 H 2.70 0.1 1 98 . 18 ASN HB3 H 2.46 0.1 1 99 . 18 ASN HD21 H 7.58 0.1 2 100 . 18 ASN HD22 H 6.88 0.1 2 101 . 19 ALA H H 7.74 0.1 1 102 . 19 ALA HA H 4.22 0.1 1 103 . 19 ALA HB H 1.50 0.1 1 104 . 20 LEU H H 8.92 0.1 1 105 . 20 LEU HA H 3.92 0.1 1 106 . 20 LEU HB2 H 1.71 0.1 2 107 . 20 LEU HB3 H 1.63 0.1 2 108 . 20 LEU HG H 1.68 0.1 1 109 . 20 LEU HD1 H 0.92 0.1 2 110 . 20 LEU HD2 H 0.88 0.1 2 111 . 21 CYS H H 7.58 0.1 1 112 . 21 CYS HA H 4.57 0.1 1 113 . 21 CYS HB2 H 3.37 0.1 1 114 . 21 CYS HB3 H 3.09 0.1 1 115 . 22 CYS H H 7.72 0.1 1 116 . 22 CYS HA H 4.73 0.1 1 117 . 22 CYS HB2 H 3.20 0.1 1 118 . 22 CYS HB3 H 3.20 0.1 1 119 . 23 ARG H H 7.67 0.1 1 120 . 23 ARG HA H 4.29 0.1 1 121 . 23 ARG HB2 H 1.84 0.1 2 122 . 23 ARG HB3 H 1.77 0.1 2 123 . 23 ARG HG2 H 1.66 0.1 1 124 . 23 ARG HG3 H 1.66 0.1 1 125 . 23 ARG HD2 H 3.12 0.1 1 126 . 23 ARG HD3 H 3.12 0.1 1 127 . 23 ARG HE H 6.99 0.1 1 128 . 24 LYS H H 8.37 0.1 1 129 . 24 LYS HA H 4.28 0.1 1 130 . 24 LYS HB2 H 1.86 0.1 2 131 . 24 LYS HB3 H 1.77 0.1 2 132 . 24 LYS HG2 H 1.45 0.1 1 133 . 24 LYS HG3 H 1.45 0.1 1 134 . 24 LYS HD2 H 1.66 0.1 1 135 . 24 LYS HD3 H 1.66 0.1 1 136 . 24 LYS HE2 H 2.98 0.1 1 137 . 24 LYS HE3 H 2.98 0.1 1 138 . 24 LYS HZ H 7.55 0.1 1 stop_ save_