data_19385 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; mu-PIIIA-2 ; _BMRB_accession_number 19385 _BMRB_flat_file_name bmr19385.str _Entry_type original _Submission_date 2013-07-23 _Accession_date 2013-07-23 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'conotoxin mu-PIIIA-2' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Ohlenschlager Oliver . . 2 Tietze Alesia . . 3 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" 141 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-08-14 original author . stop_ loop_ _Related_BMRB_accession_number _Relationship 19384 'conotoxin muPIIIA-1' stop_ _Original_release_date 2013-08-14 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Structurally diverse mu-conotoxin PIIIA isomers block sodium channel NaV 1.4' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 22407516 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Tietze Alesia A. . 2 Tietze Daniel . . 3 Ohlenschlager Oliver A. . 4 Leipold Enrico . . 5 Ullrich Florian . . 6 Kuhl Toni . . 7 Mischo Andre . . 8 Buntkowsky Gert . . 9 Gorlach Matthias . . 10 Heinemann Stefan H. . 11 Imhof Diana . . stop_ _Journal_abbreviation 'Angew. Chem. Int. Ed. Engl.' _Journal_volume 51 _Journal_issue 17 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 4058 _Page_last 4061 _Year 2012 _Details . loop_ _Keyword conotoxin NMR 'solution structure' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'conotoxin muPIIIA-2' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'conotoxin muPIIIA-2' $conotoxin_muPIIIA-2 stop_ _System_molecular_weight 2603.1 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_conotoxin_muPIIIA-2 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common conotoxin_muPIIIA-2 _Molecular_mass 2603.1 _Mol_thiol_state 'all disulfide bound' loop_ _Biological_function ; Block of voltage gated sodium channels Nav1.4 (SCN4A) mu-PIIIA-2 IC50 =103.2+/-9.9 nM ; stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 23 _Mol_residue_sequence ; ERLCCGFXKSCRSRQCKXHR CCX ; loop_ _Residue_seq_code _Residue_label 1 GLU 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 2015-02-04 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 BMRB 19384 conotoxin_muPIIIA-1 91.30 23 100.00 100.00 3.70e-02 PDB 1R9I "Nmr Solution Structure Of Piiia Toxin, Nmr, 20 Structures" 86.96 22 100.00 100.00 1.38e-01 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 C C C . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CD CD C . 0 . ? CG CG C . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HD1 HD1 H . 0 . ? HD22 HD22 H . 0 . ? HD23 HD23 H . 0 . ? HG HG H . 0 . ? HXT HXT H . 0 . ? N N N . 0 . ? O O O . 0 . ? OD1 OD1 O . 0 . ? OXT OXT O . 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 HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? N N 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 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 $conotoxin_muPIIIA-2 'Conus purpurascens' 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 $conotoxin_muPIIIA-2 'chemical synthesis' . . . . n.a. 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-2 0.9 mM 'natural abundance' H2O 90 % 'natural abundance' D2O 10 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection 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' 'data analysis' stop_ _Details . save_ save_CYANA _Saveframe_category software _Name CYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_OPAL _Saveframe_category software _Name OPAL _Version . loop_ _Vendor _Address _Electronic_address 'Luginbuhl, Guntert, Billeter and Wuthrich' . . stop_ loop_ _Task refinement stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 750 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_DQF-COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _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_ save_2D_1H-13C_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_NMR_spectrometer_expt _Saveframe_category NMR_applied_experiment _Experiment_name . _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 293 . K pH 7 . pH pressure 1 . atm 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 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 DQF-COSY' '2D 1H-1H TOCSY' '2D 1H-13C HSQC' 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-2' _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 GLU H H 7.990 0.025 1 2 1 1 GLU HA H 4.550 0.025 1 3 1 1 GLU HB2 H 2.980 0.025 2 4 1 1 GLU HB3 H 3.110 0.025 2 5 1 1 GLU HG2 H 4.280 0.025 2 6 1 1 GLU HG3 H 4.280 0.025 2 7 2 2 ARG H H 8.347 0.025 1 8 2 2 ARG HA H 4.170 0.025 1 9 2 2 ARG HB3 H 1.648 0.025 2 10 2 2 ARG HB2 H 1.648 0.025 2 11 2 2 ARG HG3 H 1.520 0.025 2 12 2 2 ARG HG2 H 1.520 0.025 2 13 2 2 ARG HD2 H 2.996 0.025 2 14 2 2 ARG HD3 H 2.996 0.025 2 15 2 2 ARG HH11 H 7.040 0.025 1 16 2 2 ARG HH12 H 7.040 0.025 1 17 3 3 LEU H H 8.198 0.025 1 18 3 3 LEU HA H 4.321 0.025 1 19 3 3 LEU HB2 H 1.540 0.025 2 20 3 3 LEU HB3 H 1.483 0.025 2 21 3 3 LEU HD1 H 0.769 0.025 2 22 3 3 LEU HD2 H 0.830 0.025 2 23 4 4 CYS H H 8.296 0.025 1 24 4 4 CYS HA H 4.470 0.025 1 25 4 4 CYS HB2 H 2.280 0.025 2 26 4 4 CYS HB3 H 2.568 0.025 2 27 5 5 CYS H H 7.926 0.025 1 28 5 5 CYS HA H 4.238 0.025 1 29 5 5 CYS HB2 H 2.880 0.025 2 30 5 5 CYS HB3 H 3.250 0.025 2 31 6 6 GLY H H 8.511 0.025 1 32 6 6 GLY HA3 H 3.779 0.025 2 33 6 6 GLY HA2 H 3.828 0.025 2 34 7 7 PHE H H 7.371 0.025 1 35 7 7 PHE HA H 4.961 0.025 1 36 7 7 PHE HB2 H 2.980 0.025 2 37 7 7 PHE HB3 H 3.084 0.025 2 38 7 7 PHE HD1 H 7.111 0.025 1 39 7 7 PHE HE1 H 7.185 0.025 1 40 7 7 PHE HZ H 7.320 0.025 1 41 7 7 PHE HE2 H 7.185 0.025 1 42 7 7 PHE HD2 H 7.111 0.025 1 43 8 8 HYP HA H 4.410 0.025 1 44 8 8 HYP HB2 H 2.050 0.025 2 45 8 8 HYP HB3 H 2.321 0.025 2 46 8 8 HYP HG H 4.610 0.025 1 47 8 8 HYP HD22 H 3.880 0.025 2 48 8 8 HYP HD23 H 3.750 0.025 2 49 9 9 LYS H H 8.787 0.025 1 50 9 9 LYS HA H 3.980 0.025 1 51 9 9 LYS HB3 H 1.920 0.025 2 52 9 9 LYS HB2 H 1.920 0.025 2 53 9 9 LYS HG2 H 1.350 0.025 2 54 9 9 LYS HG3 H 1.320 0.025 2 55 9 9 LYS HD2 H 1.840 0.025 2 56 9 9 LYS HD3 H 1.840 0.025 2 57 9 9 LYS HE2 H 2.900 0.025 2 58 9 9 LYS HE3 H 2.900 0.025 2 59 9 9 LYS HZ H 7.420 0.025 1 60 10 10 SER H H 7.765 0.025 1 61 10 10 SER HA H 4.004 0.025 1 62 10 10 SER HB2 H 3.379 0.025 2 63 10 10 SER HB3 H 3.800 0.025 2 64 11 11 CYS H H 8.137 0.025 1 65 11 11 CYS HA H 4.389 0.025 1 66 11 11 CYS HB2 H 2.880 0.025 2 67 11 11 CYS HB3 H 3.110 0.025 2 68 12 12 ARG H H 7.410 0.025 1 69 12 12 ARG HA H 4.189 0.025 1 70 12 12 ARG HB2 H 1.930 0.025 2 71 12 12 ARG HB3 H 1.930 0.025 2 72 12 12 ARG HG3 H 1.790 0.025 2 73 12 12 ARG HG2 H 1.790 0.025 2 74 12 12 ARG HD2 H 3.130 0.025 2 75 12 12 ARG HD3 H 2.910 0.025 2 76 12 12 ARG HH11 H 7.180 0.025 1 77 12 12 ARG HH12 H 7.180 0.025 1 78 13 13 SER H H 7.723 0.025 1 79 13 13 SER HA H 4.460 0.025 1 80 13 13 SER HB2 H 4.008 0.025 2 81 13 13 SER HB3 H 4.460 0.025 2 82 14 14 ARG H H 9.020 0.025 1 83 14 14 ARG HA H 3.950 0.025 1 84 14 14 ARG HB2 H 1.800 0.025 2 85 14 14 ARG HB3 H 1.870 0.025 2 86 14 14 ARG HG2 H 1.620 0.025 2 87 14 14 ARG HG3 H 1.680 0.025 2 88 14 14 ARG HD3 H 3.180 0.025 2 89 14 14 ARG HD2 H 3.180 0.025 2 90 14 14 ARG HH11 H 7.176 0.025 1 91 14 14 ARG HH12 H 7.176 0.025 1 92 15 15 GLN H H 8.557 0.025 1 93 15 15 GLN HA H 4.100 0.025 1 94 15 15 GLN HB3 H 2.020 0.025 2 95 15 15 GLN HB2 H 2.020 0.025 2 96 15 15 GLN HG2 H 2.380 0.025 2 97 15 15 GLN HG3 H 2.380 0.025 2 98 15 15 GLN HE21 H 7.146 0.025 2 99 16 16 CYS H H 7.486 0.025 1 100 16 16 CYS HA H 4.780 0.025 1 101 16 16 CYS HB2 H 2.996 0.025 2 102 16 16 CYS HB3 H 3.180 0.025 2 103 17 17 LYS H H 7.855 0.025 1 104 17 17 LYS HA H 4.110 0.025 1 105 17 17 LYS HB2 H 1.800 0.025 2 106 17 17 LYS HB3 H 1.930 0.025 2 107 17 17 LYS HG3 H 1.480 0.025 2 108 17 17 LYS HG2 H 1.480 0.025 2 109 17 17 LYS HD2 H 1.610 0.025 2 110 17 17 LYS HD3 H 1.690 0.025 2 111 17 17 LYS HE3 H 2.760 0.025 2 112 17 17 LYS HE2 H 2.760 0.025 2 113 18 18 HYP HA H 4.440 0.025 1 114 18 18 HYP HB2 H 2.340 0.025 2 115 18 18 HYP HB3 H 2.300 0.025 2 116 18 18 HYP HG H 3.240 0.025 1 117 18 18 HYP HD22 H 3.840 0.025 2 118 18 18 HYP HD23 H 3.740 0.025 2 119 19 19 HIS H H 8.180 0.025 1 120 19 19 HIS HA H 4.370 0.025 1 121 19 19 HIS HB2 H 3.280 0.025 2 122 19 19 HIS HB3 H 3.550 0.025 2 123 19 19 HIS HE1 H 7.310 0.025 1 124 20 20 ARG H H 8.980 0.025 1 125 20 20 ARG HA H 4.050 0.025 1 126 20 20 ARG HB2 H 1.850 0.025 2 127 20 20 ARG HB3 H 1.850 0.025 2 128 20 20 ARG HG2 H 1.610 0.025 2 129 20 20 ARG HG3 H 1.680 0.025 2 130 20 20 ARG HD2 H 3.270 0.025 2 131 20 20 ARG HD3 H 3.160 0.025 2 132 20 20 ARG HH11 H 7.147 0.025 1 133 20 20 ARG HH12 H 7.147 0.025 1 134 21 21 CYS H H 8.520 0.025 1 135 21 21 CYS HA H 4.530 0.025 1 136 21 21 CYS HB2 H 3.030 0.025 2 137 21 21 CYS HB3 H 3.170 0.025 2 138 22 22 CYS H H 7.920 0.025 1 139 22 22 CYS HA H 4.830 0.025 1 140 22 22 CYS HB2 H 3.080 0.025 2 141 22 22 CYS HB3 H 3.410 0.025 2 stop_ save_