data_27385 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; mu-PIIIA-9 ; _BMRB_accession_number 27385 _BMRB_flat_file_name bmr27385.str _Entry_type original _Submission_date 2018-01-24 _Accession_date 2018-01-24 _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 Tietze Daniel . . 2 Tietze Alesia A. . 3 Heimer Pascal . . 4 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" 118 "13C chemical shifts" 32 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 27382 conotoxin_muPIIIA-4 27383 conotoxin_muPIIIA-5 27384 conotoxin_muPIIIA-6 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 J. . 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-9 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label conotoxin_muPIIIA-9 $conotoxin_muPIIIA-9 stop_ _System_molecular_weight . _System_physical_state na _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_conotoxin_muPIIIA-9 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common conotoxin_muPIIIA-9 _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 _Details $conotoxin_muPIIIA-9 'Conus purpurascens' 41690 Eukaryota Metazoa Conus purpurascens 'Taxonomy ID: 41690; 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-9 '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-9 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 700 _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_ save_2D_1H-13C_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _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' '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-9 _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 HA H 4.236 0.002 1 2 1 1 PCA HB2 H 2.380 0.000 2 3 1 1 PCA HB3 H 1.884 0.000 2 4 1 1 PCA HG2 H 2.278 0.000 1 5 1 1 PCA CA C 59.278 0.000 1 6 1 1 PCA CB C 28.024 0.000 1 7 1 1 PCA CG C 31.892 0.000 1 8 2 2 ARG H H 8.324 0.002 1 9 2 2 ARG HA H 4.170 0.001 1 10 2 2 ARG HB2 H 1.679 0.002 2 11 2 2 ARG HB3 H 1.619 0.002 2 12 2 2 ARG HG2 H 1.473 0.001 2 13 2 2 ARG HG3 H 1.453 0.001 2 14 2 2 ARG HD2 H 3.052 0.003 1 15 3 3 LEU H H 8.319 0.000 1 16 3 3 LEU HA H 4.263 0.007 1 17 3 3 LEU HB2 H 1.489 0.000 1 18 3 3 LEU HD1 H 0.726 0.002 1 19 3 3 LEU HD2 H 0.726 0.002 1 20 3 3 LEU CA C 56.421 0.000 1 21 3 3 LEU CG C 24.902 0.000 1 22 3 3 LEU CD1 C 23.222 0.000 2 23 3 3 LEU CD2 C 24.863 0.000 2 24 4 4 CYS H H 8.609 0.002 1 25 4 4 CYS HA H 4.143 0.002 1 26 4 4 CYS HB2 H 3.264 0.001 2 27 4 4 CYS HB3 H 3.543 0.007 2 28 5 5 CYS H H 7.935 0.025 1 29 5 5 CYS HA H 4.876 0.000 1 30 5 5 CYS HB2 H 2.607 0.000 1 31 6 6 GLY H H 8.496 0.001 1 32 6 6 GLY HA2 H 3.749 0.001 1 33 6 6 GLY HA3 H 3.749 0.001 1 34 6 6 GLY CA C 45.109 0.000 1 35 7 7 PHE H H 8.091 0.001 1 36 7 7 PHE HA H 4.739 0.002 1 37 7 7 PHE HB2 H 2.771 0.004 2 38 7 7 PHE HB3 H 2.990 0.009 2 39 7 7 PHE HD1 H 7.128 0.001 1 40 7 7 PHE HD2 H 7.128 0.001 1 41 7 7 PHE CB C 38.635 0.000 1 42 8 8 HYP HA H 4.440 0.006 1 43 8 8 HYP HB2 H 2.202 0.003 2 44 8 8 HYP HB3 H 1.916 0.005 2 45 8 8 HYP HG H 4.454 0.001 1 46 8 8 HYP HD22 H 3.754 0.009 2 47 8 8 HYP HD23 H 3.576 0.004 2 48 8 8 HYP CA C 61.721 0.000 1 49 8 8 HYP CG C 72.550 0.000 1 50 8 8 HYP CD C 58.224 0.000 1 51 9 9 LYS H H 8.531 0.010 1 52 9 9 LYS HA H 4.152 0.002 1 53 9 9 LYS HB2 H 1.662 0.003 2 54 9 9 LYS HB3 H 1.739 0.005 2 55 9 9 LYS HG2 H 1.394 0.004 2 56 9 9 LYS HG3 H 1.338 0.005 2 57 9 9 LYS HD2 H 1.576 0.006 1 58 9 9 LYS HD3 H 1.576 0.006 1 59 9 9 LYS HE2 H 2.881 0.003 1 60 9 9 LYS HE3 H 2.881 0.003 1 61 9 9 LYS CA C 56.922 0.000 1 62 9 9 LYS CB C 32.672 0.000 1 63 9 9 LYS CE C 42.096 0.000 1 64 10 10 SER H H 8.149 0.002 1 65 10 10 SER HA H 4.265 0.003 1 66 10 10 SER HB2 H 3.715 0.003 2 67 10 10 SER HB3 H 3.742 0.000 2 68 10 10 SER CA C 58.405 0.000 1 69 10 10 SER CB C 63.724 0.000 1 70 11 11 CYS H H 8.319 0.000 1 71 11 11 CYS HA H 4.589 0.002 1 72 11 11 CYS HB2 H 3.069 0.002 2 73 11 11 CYS HB3 H 2.983 0.001 2 74 11 11 CYS CB C 41.978 0.000 1 75 12 12 ARG H H 8.624 0.001 1 76 12 12 ARG HA H 4.311 0.003 1 77 12 12 ARG HB2 H 1.844 0.005 2 78 12 12 ARG HB3 H 1.595 0.003 2 79 12 12 ARG HG2 H 1.491 0.005 2 80 12 12 ARG HG3 H 1.493 0.004 2 81 12 12 ARG HD2 H 3.059 0.002 1 82 12 12 ARG CA C 56.177 0.000 1 83 13 13 SER H H 7.783 0.002 1 84 13 13 SER HA H 4.364 0.001 1 85 13 13 SER HB2 H 3.888 0.002 2 86 13 13 SER HB3 H 3.782 0.001 2 87 13 13 SER CA C 57.632 0.000 1 88 13 13 SER CB C 64.065 0.000 1 89 14 14 ARG H H 8.299 0.001 1 90 14 14 ARG HA H 4.018 0.001 1 91 14 14 ARG HB2 H 1.748 0.002 1 92 14 14 ARG HB3 H 1.748 0.002 1 93 14 14 ARG HG2 H 1.527 0.005 1 94 14 14 ARG HG3 H 1.526 0.005 1 95 14 14 ARG HD2 H 3.069 0.002 1 96 14 14 ARG CA C 57.706 0.000 1 97 15 15 GLN H H 8.099 0.002 1 98 15 15 GLN HA H 4.174 0.013 1 99 15 15 GLN HB2 H 1.956 0.002 2 100 15 15 GLN HB3 H 1.850 0.004 2 101 15 15 GLN HG2 H 2.207 0.003 2 102 15 15 GLN HG3 H 2.208 0.002 2 103 15 15 GLN CA C 56.314 0.000 1 104 15 15 GLN CB C 28.898 0.000 1 105 15 15 GLN CG C 33.885 0.000 1 106 16 16 CYS H H 7.973 0.002 1 107 16 16 CYS HA H 4.461 0.002 1 108 16 16 CYS HB2 H 3.076 0.003 2 109 16 16 CYS HB3 H 2.950 0.004 2 110 16 16 CYS CB C 41.605 0.000 1 111 17 17 LYS H H 8.070 0.001 1 112 17 17 LYS HA H 4.453 0.002 1 113 17 17 LYS HB2 H 1.576 0.006 2 114 17 17 LYS HB3 H 1.656 0.005 2 115 17 17 LYS HG2 H 1.343 0.006 2 116 17 17 LYS HG3 H 1.298 0.008 2 117 17 17 LYS HD2 H 1.544 0.005 2 118 17 17 LYS HD3 H 1.541 0.004 2 119 17 17 LYS HE2 H 2.837 0.000 1 120 17 17 LYS HE3 H 2.837 0.000 1 121 17 17 LYS CB C 32.450 0.000 1 122 17 17 LYS CE C 41.997 0.000 1 123 18 18 HYP HA H 4.391 0.002 1 124 18 18 HYP HB2 H 2.169 0.005 2 125 18 18 HYP HB3 H 1.827 0.003 2 126 18 18 HYP HG H 4.449 0.002 1 127 18 18 HYP HD22 H 3.639 0.003 2 128 18 18 HYP HD23 H 3.726 0.005 2 129 18 18 HYP CA C 61.566 0.000 1 130 18 18 HYP CD C 58.294 0.000 1 131 19 19 HIS H H 8.659 0.003 1 132 19 19 HIS HA H 4.522 0.003 1 133 19 19 HIS HB2 H 3.073 0.005 1 134 19 19 HIS HB3 H 3.073 0.005 1 135 19 19 HIS HD2 H 7.157 0.000 1 136 19 19 HIS CA C 55.511 0.000 1 137 19 19 HIS CB C 29.340 0.000 1 138 20 20 ARG H H 8.349 0.000 1 139 20 20 ARG HA H 4.176 0.003 1 140 20 20 ARG HB2 H 1.658 0.001 2 141 20 20 ARG HB3 H 1.588 0.003 2 142 20 20 ARG HG2 H 1.468 0.002 1 143 20 20 ARG HG3 H 1.468 0.002 1 144 20 20 ARG HD2 H 3.047 0.008 1 145 21 21 CYS H H 8.158 0.003 1 146 21 21 CYS HA H 4.813 0.004 1 147 21 21 CYS HB2 H 3.286 0.000 2 148 21 21 CYS HB3 H 3.475 0.000 2 149 22 22 CYS H H 8.669 0.002 1 150 22 22 CYS HA H 3.808 0.000 1 stop_ save_