data_25174 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Non-reducible analogues of alpha-conotoxin RgIA: [2,8]-cis dicarba RgIA ; _BMRB_accession_number 25174 _BMRB_flat_file_name bmr25174.str _Entry_type original _Submission_date 2014-08-26 _Accession_date 2014-08-26 _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 Chhabra Sandeep . . 2 Robinson Sam . . 3 Norton Ray . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 72 "13C chemical shifts" 37 "15N chemical shifts" 11 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-09-28 update BMRB 'update entry citation' 2014-11-24 original author 'original release' stop_ _Original_release_date 2016-09-28 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Dicarba Analogues of alpha-Conotoxin RgIA. Structure, Stability and Activity at Potential Pain Targets ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 25393758 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 chhabra sandeep . . 2 Belgi Alessia . . 3 Bartels Peter . . 4 Robinson Samuel D. . 5 Kompella Shiva N. . 6 Hung Andrew . . 7 Callaghan Brid P. . 8 Adams David J. . 9 Robinson Andrea J. . 10 Norton Raymond S. . stop_ _Journal_abbreviation 'J. Med. Chem' _Journal_volume 57 _Journal_issue 23 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 9933 _Page_last 9944 _Year 2014 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Non-reducible analogues of alpha-conotoxin RgIA: [2,8]-cis dicarba RgIA' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label Alpha-conotoxin_RgIA $Alpha-conotoxin_RgIA stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Alpha-conotoxin_RgIA _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Alpha-conotoxin_RgIA _Molecular_mass 1542.793 _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 13 _Mol_residue_sequence ; GXCSDPRXRYRCR ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 GLY 2 2 ABA 3 3 CYS 4 4 SER 5 5 ASP 6 6 PRO 7 7 ARG 8 8 ABA 9 9 ARG 10 10 TYR 11 11 ARG 12 12 CYS 13 13 ARG stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_ABA _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 'ALPHA-AMINOBUTYRIC ACID' _BMRB_code ABA _PDB_code ABA _Standard_residue_derivative . _Molecular_mass 103.120 _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 . ? OXT OXT O . 0 . ? H H H . 0 . ? HN2 HN2 H . 0 . ? HA HA H . 0 . ? HB3 HB3 H . 0 . ? HB2 HB2 H . 0 . ? HG1 HG1 H . 0 . ? HG3 HG3 H . 0 . ? HG2 HG2 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 H ? ? SING N HN2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB3 ? ? SING CB HB2 ? ? SING CG HG1 ? ? SING CG HG3 ? ? SING CG HG2 ? ? 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 $Alpha-conotoxin_RgIA 'crown cone' 101314 Eukaryota Metazoa Conus regius 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 $Alpha-conotoxin_RgIA 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $Alpha-conotoxin_RgIA 500 uM 'natural abundance' D2O 100 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CYANA _Saveframe_category software _Name CYANA _Version 3.0 loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_X-PLOR_NIH _Saveframe_category software _Name X-PLOR_NIH _Version 2.35 loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . 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 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_2 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_2 save_ save_2D_1H-15N_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_2 save_ save_2D_DQF-COSY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_2 save_ save_2D_1H-1H_NOESY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 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' 0.003 0.002 M pH 3.0 . pH pressure 1 . atm temperature 298 . 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 dioxane C 13 'methylene protons' ppm 3.75 internal indirect . . . 0.251449530 dioxane H 1 'methylene protons' ppm 3.75 internal direct . . . 1.000000000 dioxane N 15 'methylene protons' ppm 3.75 internal indirect . . . 0.10132918 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 TOCSY' '2D 1H-15N HSQC' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name Alpha-conotoxin_RgIA _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 GLY HA2 H 3.931 0.006 . 2 1 1 GLY HA3 H 3.962 0.004 . 3 1 1 GLY CA C 43.363 0.000 . 4 2 2 ABA CA C 56.334 0.000 . 5 2 2 ABA CB C 31.669 0.032 . 6 2 2 ABA CG C 129.248 0.000 . 7 2 2 ABA H H 8.767 0.002 . 8 2 2 ABA HA H 4.667 0.003 . 9 2 2 ABA HB2 H 2.602 0.004 . 10 2 2 ABA HB3 H 2.728 0.005 . 11 2 2 ABA HG1 H 5.634 0.003 . 12 2 2 ABA HG2 H 5.634 0.003 . 13 2 2 ABA HG3 H 5.634 0.003 . 14 2 2 ABA N N 119.007 0.000 . 15 3 3 CYS H H 8.158 0.002 . 16 3 3 CYS HA H 4.452 0.003 . 17 3 3 CYS HB2 H 3.380 0.003 . 18 3 3 CYS HB3 H 2.986 0.002 . 19 3 3 CYS CA C 56.965 0.000 . 20 3 3 CYS CB C 41.372 0.043 . 21 3 3 CYS N N 115.656 0.000 . 22 4 4 SER H H 8.554 0.004 . 23 4 4 SER HA H 4.369 0.000 . 24 4 4 SER HB2 H 3.980 0.004 . 25 4 4 SER CA C 58.608 0.000 . 26 4 4 SER CB C 62.908 0.000 . 27 4 4 SER N N 114.552 0.000 . 28 5 5 ASP H H 7.937 0.002 . 29 5 5 ASP HA H 5.096 0.002 . 30 5 5 ASP HB2 H 3.083 0.007 . 31 5 5 ASP HB3 H 2.788 0.009 . 32 5 5 ASP CA C 50.787 0.000 . 33 5 5 ASP CB C 40.748 0.001 . 34 5 5 ASP N N 121.374 0.000 . 35 6 6 PRO HA H 4.320 0.007 . 36 6 6 PRO HB2 H 2.398 0.002 . 37 6 6 PRO HB3 H 1.964 0.007 . 38 6 6 PRO HG2 H 2.035 0.010 . 39 6 6 PRO HG3 H 2.064 0.005 . 40 6 6 PRO HD2 H 3.921 0.005 . 41 6 6 PRO CA C 64.894 0.000 . 42 6 6 PRO CB C 32.316 0.006 . 43 6 6 PRO CG C 27.454 0.000 . 44 6 6 PRO CD C 51.163 0.000 . 45 7 7 ARG H H 8.115 0.002 . 46 7 7 ARG HA H 4.217 0.002 . 47 7 7 ARG HB2 H 1.891 0.003 . 48 7 7 ARG HB3 H 1.779 0.005 . 49 7 7 ARG HG2 H 1.644 0.002 . 50 7 7 ARG HD2 H 3.214 0.002 . 51 7 7 ARG HE H 7.418 0.002 . 52 7 7 ARG CA C 56.607 0.052 . 53 7 7 ARG CB C 30.225 0.000 . 54 7 7 ARG CG C 27.295 0.000 . 55 7 7 ARG N N 115.647 0.000 . 56 8 8 ABA CA C 56.058 0.056 . 57 8 8 ABA CB C 32.389 0.000 . 58 8 8 ABA CG C 131.485 0.000 . 59 8 8 ABA H H 7.776 0.002 . 60 8 8 ABA HA H 4.275 0.005 . 61 8 8 ABA HB2 H 2.593 0.008 . 62 8 8 ABA HG1 H 5.626 0.003 . 63 8 8 ABA HG2 H 5.626 0.003 . 64 8 8 ABA HG3 H 5.626 0.003 . 65 8 8 ABA N N 121.042 0.000 . 66 9 9 ARG H H 8.293 0.002 . 67 9 9 ARG HA H 4.127 0.004 . 68 9 9 ARG HB2 H 1.718 0.003 . 69 9 9 ARG HB3 H 1.671 0.002 . 70 9 9 ARG HG2 H 1.479 0.004 . 71 9 9 ARG HD2 H 3.112 0.002 . 72 9 9 ARG HE H 7.083 0.002 . 73 9 9 ARG CA C 57.118 0.004 . 74 9 9 ARG CB C 29.696 0.014 . 75 9 9 ARG CG C 26.892 0.000 . 76 9 9 ARG N N 122.240 0.000 . 77 10 10 TYR H H 7.412 0.002 . 78 10 10 TYR HA H 4.623 0.003 . 79 10 10 TYR HB2 H 3.112 0.005 . 80 10 10 TYR HB3 H 2.928 0.007 . 81 10 10 TYR HD1 H 7.125 0.003 . 82 10 10 TYR HD2 H 7.125 0.003 . 83 10 10 TYR HE1 H 6.870 0.003 . 84 10 10 TYR HE2 H 6.870 0.003 . 85 10 10 TYR CA C 56.261 0.000 . 86 10 10 TYR CB C 38.916 0.032 . 87 10 10 TYR CD1 C 133.463 0.000 . 88 10 10 TYR CD2 C 133.463 0.000 . 89 10 10 TYR CE1 C 118.203 0.000 . 90 10 10 TYR CE2 C 118.203 0.000 . 91 10 10 TYR N N 118.230 0.000 . 92 11 11 ARG H H 8.268 0.002 . 93 11 11 ARG HA H 4.264 0.002 . 94 11 11 ARG HB2 H 1.778 0.004 . 95 11 11 ARG HB3 H 1.811 0.002 . 96 11 11 ARG HG2 H 1.559 0.003 . 97 11 11 ARG HD2 H 3.181 0.002 . 98 11 11 ARG HE H 7.160 0.002 . 99 11 11 ARG CA C 56.149 0.000 . 100 11 11 ARG CB C 30.598 0.000 . 101 11 11 ARG CG C 27.128 0.000 . 102 11 11 ARG N N 120.334 0.000 . 103 12 12 CYS H H 8.514 0.002 . 104 12 12 CYS HA H 4.613 0.002 . 105 12 12 CYS HB2 H 3.196 0.004 . 106 12 12 CYS HB3 H 3.109 0.005 . 107 12 12 CYS CA C 56.492 0.000 . 108 12 12 CYS CB C 43.258 0.015 . 109 12 12 CYS N N 121.083 0.000 . 110 13 13 ARG H H 8.181 0.002 . 111 13 13 ARG HA H 4.271 0.000 . 112 13 13 ARG HB2 H 1.895 0.003 . 113 13 13 ARG HB3 H 1.767 0.003 . 114 13 13 ARG HG2 H 1.623 0.007 . 115 13 13 ARG HD2 H 3.198 0.002 . 116 13 13 ARG HE H 7.182 0.002 . 117 13 13 ARG CA C 57.404 1.232 . 118 13 13 ARG CB C 30.970 0.009 . 119 13 13 ARG CG C 27.242 0.000 . 120 13 13 ARG N N 126.012 0.000 . stop_ save_