data_19102 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR and Mass Spectrometric Studies of M-2 Branch Mini-M Conotoxins from Indian Cone Snails ; _BMRB_accession_number 19102 _BMRB_flat_file_name bmr19102.str _Entry_type original _Submission_date 2013-03-18 _Accession_date 2013-03-18 _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 Sarma Siddhartha . . 2 'R. P.' Rajesh . . 3 Ganesan 'Senthil Kumar' . . 4 S Sudarshlal . . 5 V Sabaressh . . 6 'Gowd K.' Hanume . . 7 Gupta Kallol . . 8 'K. S.' Krishnan . . 9 Padmanabhan Balaram . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 67 "13C chemical shifts" 36 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2014-04-14 original author . stop_ _Original_release_date 2014-04-14 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'NMR and Mass Spectrometric Studies of M-2 Branch Mini-M Conotoxins from Indian Cone Snails' _Citation_status 'in preparation' _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Sarma Siddhartha . . stop_ _Journal_abbreviation 'Not known' _Journal_volume . _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year . _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'M-2 Branch Mini-M Conotoxins' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'M-2 Branch Mini-M Conotoxins' $conotoxin 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_conotoxin _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity _Molecular_mass 1454.814 _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 15 _Mol_residue_sequence CCRLACGLGCHXCCX loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 CYS 2 2 CYS 3 3 ARG 4 4 LEU 5 5 ALA 6 6 CYS 7 7 GLY 8 8 LEU 9 9 GLY 10 10 CYS 11 11 HIS 12 12 HYP 13 13 CYS 14 14 CYS 15 15 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_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $conotoxin Gastropods 101286 Eukaryota Metazoa Conus araneosus 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 'purified from the natural source' . Conus araneosus . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_ar1446 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $conotoxin 0.2 mM 'natural abundance' methanol 100 % 'natural abundance' stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_DQF-COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $ar1446 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $ar1446 save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $ar1446 save_ save_2D_1H-13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $ar1446 save_ ####################### # Sample conditions # ####################### save_ar1446_sample_conditions _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' na . 'Not defined' pH na . 'Not defined' pressure 1 . atm temperature 303 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_methanol _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 methanol C 13 'methyl carbon' ppm 49.0 internal direct . . . 0.25144953 methanol H 1 'methyl protons' ppm 3.30 internal direct . . . 1.00000000 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_ar1446_assigned_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D DQF-COSY' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $ar1446 stop_ _Sample_conditions_label $ar1446_sample_conditions _Chem_shift_reference_set_label $methanol _Mol_system_component_name 'M-2 Branch Mini-M Conotoxins' _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 CYS HA H 4.16 0.01 1 2 1 1 CYS HB2 H 3.13 0.01 2 3 1 1 CYS HB3 H 2.98 0.01 2 4 1 1 CYS CA C 52.48 0.02 1 5 1 1 CYS CB C 40.25 0.02 1 6 2 2 CYS H H 8.81 0.01 1 7 2 2 CYS HA H 4.73 0.01 1 8 2 2 CYS HB2 H 3.47 0.01 2 9 2 2 CYS HB3 H 3.35 0.01 2 10 2 2 CYS CA C 56.43 0.02 1 11 2 2 CYS CB C 45.09 0.02 1 12 3 3 ARG H H 8.93 0.01 1 13 3 3 ARG HA H 4.40 0.01 1 14 3 3 ARG HB2 H 1.85 0.01 2 15 3 3 ARG HB3 H 1.73 0.01 2 16 3 3 ARG HG2 H 1.70 0.01 2 17 3 3 ARG HG3 H 1.64 0.01 2 18 3 3 ARG HD2 H 3.20 0.01 2 19 3 3 ARG HD3 H 3.16 0.01 2 20 3 3 ARG CA C 55.15 0.02 1 21 3 3 ARG CB C 30.39 0.02 1 22 3 3 ARG CG C 26.40 0.02 1 23 3 3 ARG CD C 41.63 0.02 1 24 4 4 LEU H H 8.00 0.01 1 25 4 4 LEU HA H 4.32 0.01 1 26 4 4 LEU HB2 H 1.69 0.01 2 27 4 4 LEU HB3 H 1.63 0.01 2 28 4 4 LEU HG H 1.63 0.01 2 29 4 4 LEU HD1 H 0.95 0.01 1 30 4 4 LEU HD2 H 0.93 0.01 1 31 4 4 LEU CA C 53.81 0.02 1 32 4 4 LEU CB C 41.62 0.02 1 33 4 4 LEU CG C 25.72 0.02 1 34 4 4 LEU CD1 C 23.10 0.02 1 35 4 4 LEU CD2 C 21.47 0.02 1 36 5 5 ALA H H 7.99 0.01 1 37 5 5 ALA HA H 4.168 0.01 1 38 5 5 ALA HB H 1.31 0.01 1 39 5 5 ALA CA C 50.08 0.02 1 40 5 5 ALA CB C 16.98 0.02 1 41 6 6 CYS H H 8.18 0.01 1 42 6 6 CYS HA H 5.13 0.01 1 43 6 6 CYS HB2 H 3.25 0.01 2 44 6 6 CYS HB3 H 3.07 0.01 2 45 6 6 CYS CA C 54.20 0.02 1 46 6 6 CYS CB C 40.85 0.02 1 47 7 7 GLY H H 8.350 0.01 1 48 7 7 GLY HA2 H 4.38 0.01 2 49 7 7 GLY HA3 H 3.80 0.01 2 50 7 7 GLY CA C 43.32 0.02 1 51 8 8 LEU H H 8.98 0.01 1 52 8 8 LEU HA H 3.99 0.01 1 53 8 8 LEU HB2 H 1.61 0.01 2 54 8 8 LEU HB3 H 1.61 0.01 2 55 8 8 LEU HG H 1.72 0.01 1 56 8 8 LEU HD1 H 0.96 0.01 2 57 8 8 LEU HD2 H 0.89 0.01 2 58 8 8 LEU CA C 56.41 0.02 1 59 8 8 LEU CB C 40.72 0.02 1 60 8 8 LEU CG C 25.47 0.02 1 61 8 8 LEU CD1 C 22.705 0.02 2 62 8 8 LEU CD2 C 21.76 0.02 2 63 9 9 GLY H H 8.38 0.01 1 64 9 9 GLY HA2 H 4.14 0.01 2 65 9 9 GLY HA3 H 3.60 0.01 2 66 9 9 GLY CA C 43.34 0.02 1 67 10 10 CYS H H 7.41 0.01 1 68 10 10 CYS HA H 4.61 0.01 1 69 10 10 CYS HB2 H 3.57 0.01 2 70 10 10 CYS HB3 H 2.48 0.01 2 71 10 10 CYS CA C 57.67 0.02 1 72 10 10 CYS CB C 36.24 0.02 1 73 11 11 HIS H H 8.33 0.01 1 74 11 11 HIS HA H 4.79 0.01 1 75 11 11 HIS HB2 H 3.61 0.01 2 76 11 11 HIS HB3 H 3.15 0.01 2 77 11 11 HIS HD2 H 7.40 0.01 1 78 11 11 HIS HE1 H 8.78 0.01 1 79 11 11 HIS CA C 52.09 0.02 1 80 11 11 HIS CB C 26.51 0.02 1 81 12 12 HYP CA C 58.72 0.02 1 82 12 12 HYP CB C 41.92 0.02 1 83 12 12 HYP CD C 56.81 0.02 1 84 12 12 HYP CG C 68.76 0.02 1 85 12 12 HYP HA H 4.87 0.01 1 86 12 12 HYP HB2 H 2.60 0.01 2 87 12 12 HYP HB3 H 2.16 0.01 2 88 12 12 HYP HD22 H 3.77 0.01 2 89 12 12 HYP HD23 H 3.55 0.01 2 90 12 12 HYP HG H 4.46 0.01 1 91 13 13 CYS H H 9.57 0.01 1 92 13 13 CYS HA H 5.09 0.01 1 93 13 13 CYS HB2 H 3.36 0.01 2 94 13 13 CYS HB3 H 3.21 0.01 2 95 13 13 CYS CA C 54.25 0.02 1 96 13 13 CYS CB C 39.49 0.02 1 97 14 14 CYS HA H 4.64 0.01 1 98 14 14 CYS HB2 H 2.92 0.01 2 99 14 14 CYS HB3 H 3.14 0.01 2 100 14 14 CYS CA C 53.06 0.02 1 101 14 14 CYS CB C 40.26 0.02 1 102 15 15 NH2 HN1 H 7.64 0.01 1 103 15 15 NH2 HN2 H 7.25 0.01 1 stop_ save_