data_27382 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; mu-PIIIA-4 ; _BMRB_accession_number 27382 _BMRB_flat_file_name bmr27382.str _Entry_type original _Submission_date 2018-01-23 _Accession_date 2018-01-23 _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 Heimer Pascal . . 2 Tietze Daniel . . 3 Tietze Alesia A. . 4 Ohlenschlaeger Oliver . . 5 Imhof Diana . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 119 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2018-03-23 update BMRB 'update entry citation' 2018-02-23 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 27379 conotoxin_muPIIIA-3 27383 conotoxin_muPIIIA-5 27384 conotoxin_muPIIIA-6 27385 conotoxin_muPIIIA-9 27386 conotoxin_muPIIIA-11 27388 conotoxin_muPIIIA-8 27389 conotoxin_muPIIIA-10 27390 conotoxin_muPIIIA-15 27391 conotoxin_muPIIIA-14 stop_ _Original_release_date 2018-01-24 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Conformational mu-Conotoxin PIIIA Isomers Revisited: Impact of Cysteine Pairing on Disulfide-Bond Assignment and Structure Elucidation ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 29397705 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Heimer Pascal . . 2 Tietze Alesia A. . 3 Baeuml Charlotte A. . 4 Resemann Anja . . 5 Mayer Franz . . 6 Suckau Detlev . . 7 Ohlenschlaeger Oliver . . 8 Tietze Daniel . . 9 Imhof Diana . . stop_ _Journal_abbreviation 'Anal. Chem.' _Journal_volume 90 _Journal_issue 5 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 3321 _Page_last 3327 _Year 2018 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name conotoxin_muPIIIA-4 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label conotoxin_muPIIIA-4 $conotoxin_muPIIIA-4 stop_ _System_molecular_weight 2603.1 _System_physical_state na _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_conotoxin_muPIIIA-4 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common conotoxin_muPIIIA-4 _Molecular_mass 2603.1 _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 23 _Mol_residue_sequence ; XRLCCGFXKSCRSRQCKXHR CCX ; loop_ _Residue_seq_code _Residue_label 1 PCA 2 ARG 3 LEU 4 CYS 5 CYS 6 GLY 7 PHE 8 HYP 9 LYS 10 SER 11 CYS 12 ARG 13 SER 14 ARG 15 GLN 16 CYS 17 LYS 18 HYP 19 HIS 20 ARG 21 CYS 22 CYS 23 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . 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 NH2 _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _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 . ? 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_ save_chem_comp_PCA _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 'PYROGLUTAMIC ACID' _BMRB_code PCA _PDB_code PCA _Standard_residue_derivative . _Molecular_mass 129.114 _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 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? OE OE O . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 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 CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? DOUB CD OE ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Gene_mnemonic _Details $conotoxin_muPIIIA-4 'Conus purpurascens' 41690 Eukaryota Metazoa Conus purpurascens 'Conus purpurascens' 'Taxonomy ID: 41690 Superkingdom: Eukaryota Kingdom: Metazoa.' 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 $conotoxin_muPIIIA-4 '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 $conotoxin_muPIIIA-4 0.5 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version 3.1 loop_ _Vendor _Address _Electronic_address Bruker . . stop_ loop_ _Task collection stop_ _Details . save_ save_CCPNMR _Saveframe_category software _Name CCPNMR _Version 2.4 loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_Yasara _Saveframe_category software _Name Yasara _Version . loop_ _Vendor _Address _Electronic_address 'Yasara Biosciences GmbH' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 . M pH 7.4 . pH pressure 1 . atm temperature 293 . 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 na indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 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 . loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-1H TOCSY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name conotoxin_muPIIIA-4 _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 1 PCA H H 7.767 0.000 1 2 1 1 PCA HA H 4.212 0.004 1 3 1 1 PCA HB2 H 2.380 0.000 1 4 2 2 ARG H H 8.256 0.002 1 5 2 2 ARG HA H 4.189 0.001 1 6 2 2 ARG HB2 H 1.658 0.001 2 7 2 2 ARG HB3 H 1.600 0.000 2 8 2 2 ARG HG2 H 1.513 0.002 1 9 2 2 ARG HD2 H 3.069 0.001 1 10 2 2 ARG HD3 H 3.069 0.001 1 11 3 3 LEU H H 8.329 0.003 1 12 3 3 LEU HA H 4.253 0.003 1 13 3 3 LEU HB2 H 1.641 0.005 2 14 3 3 LEU HB3 H 1.483 0.009 2 15 3 3 LEU HD1 H 0.722 0.000 1 16 3 3 LEU HD2 H 0.722 0.000 1 17 4 4 CYS H H 8.609 0.002 1 18 4 4 CYS HA H 4.148 0.003 1 19 4 4 CYS HB2 H 3.269 0.008 2 20 4 4 CYS HB3 H 3.546 0.002 2 21 5 5 CYS H H 7.936 0.023 1 22 5 5 CYS HA H 4.909 0.001 1 23 5 5 CYS HB2 H 2.586 0.005 2 24 5 5 CYS HB3 H 3.310 0.005 2 25 6 6 GLY H H 8.498 0.003 1 26 6 6 GLY HA2 H 3.762 0.005 2 27 6 6 GLY HA3 H 3.751 0.003 2 28 7 7 PHE H H 8.099 0.011 1 29 7 7 PHE HA H 4.753 0.002 1 30 7 7 PHE HB2 H 2.990 0.004 2 31 7 7 PHE HB3 H 2.774 0.003 2 32 8 8 HYP HA H 4.446 0.001 1 33 8 8 HYP HB2 H 2.203 0.003 2 34 8 8 HYP HB3 H 1.915 0.006 2 35 8 8 HYP HG H 4.458 0.003 1 36 8 8 HYP HD22 H 3.572 0.004 2 37 8 8 HYP HD23 H 3.756 0.003 2 38 9 9 LYS H H 8.526 0.001 1 39 9 9 LYS HA H 4.138 0.005 1 40 9 9 LYS HB2 H 1.737 0.002 2 41 9 9 LYS HB3 H 1.667 0.002 2 42 9 9 LYS HG2 H 1.365 0.008 2 43 9 9 LYS HG3 H 1.390 0.002 2 44 9 9 LYS HD2 H 1.580 0.005 1 45 9 9 LYS HD3 H 1.580 0.005 1 46 9 9 LYS HE2 H 2.887 0.001 1 47 9 9 LYS HE3 H 2.887 0.001 1 48 10 10 SER H H 8.152 0.002 1 49 10 10 SER HA H 4.276 0.003 1 50 10 10 SER HB2 H 3.712 0.002 2 51 10 10 SER HB3 H 3.738 0.002 2 52 11 11 CYS H H 8.308 0.004 1 53 11 11 CYS HA H 4.595 0.003 1 54 11 11 CYS HB2 H 3.064 0.005 2 55 11 11 CYS HB3 H 2.992 0.003 2 56 12 12 ARG H H 8.624 0.003 1 57 12 12 ARG HA H 4.306 0.002 1 58 12 12 ARG HB2 H 1.838 0.002 2 59 12 12 ARG HB3 H 1.600 0.008 2 60 12 12 ARG HG2 H 1.480 0.002 1 61 12 12 ARG HG3 H 1.480 0.002 1 62 12 12 ARG HD2 H 3.062 0.000 1 63 12 12 ARG HD3 H 3.062 0.000 1 64 12 12 ARG HE H 7.057 0.000 1 65 13 13 SER H H 7.790 0.002 1 66 13 13 SER HA H 4.362 0.005 1 67 13 13 SER HB2 H 3.888 0.003 2 68 13 13 SER HB3 H 3.782 0.005 2 69 14 14 ARG H H 8.294 0.003 1 70 14 14 ARG HA H 4.019 0.003 1 71 14 14 ARG HB2 H 1.748 0.001 1 72 14 14 ARG HB3 H 1.748 0.001 1 73 14 14 ARG HG2 H 1.521 0.001 1 74 14 14 ARG HG3 H 1.521 0.001 1 75 14 14 ARG HD2 H 3.071 0.002 1 76 14 14 ARG HD3 H 3.071 0.002 1 77 15 15 GLN H H 8.095 0.002 1 78 15 15 GLN HA H 4.166 0.003 1 79 15 15 GLN HB2 H 1.850 0.003 2 80 15 15 GLN HB3 H 1.956 0.002 2 81 15 15 GLN HG2 H 2.208 0.001 2 82 15 15 GLN HG3 H 2.210 0.003 2 83 15 15 GLN HE21 H 7.058 0.000 1 84 16 16 CYS H H 7.973 0.003 1 85 16 16 CYS HA H 4.457 0.001 1 86 16 16 CYS HB2 H 2.945 0.000 2 87 16 16 CYS HB3 H 3.079 0.000 2 88 17 17 LYS H H 8.077 0.004 1 89 17 17 LYS HA H 4.449 0.002 1 90 17 17 LYS HB2 H 1.575 0.002 2 91 17 17 LYS HB3 H 1.661 0.003 2 92 17 17 LYS HG2 H 1.335 0.004 2 93 17 17 LYS HG3 H 1.316 0.021 2 94 17 17 LYS HD2 H 1.540 0.001 1 95 17 17 LYS HD3 H 1.540 0.001 1 96 17 17 LYS HE2 H 2.841 0.001 1 97 17 17 LYS HE3 H 2.841 0.001 1 98 18 18 HYP HA H 4.390 0.006 1 99 18 18 HYP HB2 H 1.828 0.002 2 100 18 18 HYP HB3 H 2.178 0.007 2 101 18 18 HYP HG H 4.450 0.000 1 102 18 18 HYP HD22 H 3.721 0.004 2 103 18 18 HYP HD23 H 3.638 0.004 2 104 19 19 HIS H H 8.631 0.006 1 105 19 19 HIS HA H 4.515 0.002 1 106 19 19 HIS HB2 H 3.067 0.000 1 107 19 19 HIS HB3 H 3.067 0.000 1 108 20 20 ARG H H 8.327 0.002 1 109 20 20 ARG HA H 4.176 0.002 1 110 20 20 ARG HB2 H 1.755 0.001 2 111 20 20 ARG HB3 H 1.661 0.006 2 112 20 20 ARG HG2 H 1.489 0.000 1 113 20 20 ARG HG3 H 1.489 0.001 1 114 20 20 ARG HD2 H 3.067 0.001 1 115 21 21 CYS H H 8.156 0.003 1 116 21 21 CYS HB2 H 3.481 0.009 2 117 21 21 CYS HB3 H 3.281 0.000 2 118 22 22 CYS H H 8.675 0.000 1 119 22 22 CYS HA H 3.814 0.000 1 stop_ save_