data_6880 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H, 13C and 15N chemical shift assignments of Schistocerca gregaria chymotrypsin inhibitor at pH=6.0 ; _BMRB_accession_number 6880 _BMRB_flat_file_name bmr6880.str _Entry_type original _Submission_date 2005-10-28 _Accession_date 2005-10-28 _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 Gaspari Zoltan . . 2 Szenthe Borbala . . 3 Patthy Andras . . 4 Westler William M. . 5 Graf Laszlo . . 6 Perczel Andras . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 heteronucl_NOE 1 T1_relaxation 1 T2_relaxation 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 81 "15N chemical shifts" 23 "T1 relaxation values" 23 "T2 relaxation values" 23 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2005-12-14 original author 'original release' 2006-04-14 update author 'update citation' 2007-11-15 update BMRB 'complete entry citation' stop_ loop_ _Related_BMRB_accession_number _Relationship 5272 '1H chemical shift assignments for Schistocerca gregaria chymotrypsin inhibitor' 5273 '1H chemical shift assignments for SGCI[L30R, K31M]' 5274 '1H Chemical shift assignments of Schistocerca gregaria trypsin inhibitor' 6881 '1H and 15N chemical shift assignments of Schistocerca gregaria chymotrypsin inhibitor complexed with bovine chymotrypsin' stop_ _Original_release_date 2005-10-28 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Local binding with globally distributed changes in a small protease inhibitor upon enzyme binding ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 16623717 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Gaspari Zoltan . . 2 Szenthe Borbala . . 3 Patthy Andras . . 4 Westler William M. . 5 Graf Laszlo . . 6 Perczel Andras . . stop_ _Journal_abbreviation 'FEBS J.' _Journal_volume 273 _Journal_issue 8 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1831 _Page_last 1842 _Year 2006 _Details . loop_ _Keyword SGCI Schistocerca 'protease inhibitor' stop_ save_ ################################## # Molecular system description # ################################## save_system_SGCI _Saveframe_category molecular_system _Mol_system_name 'Schistocerca gregaria chymotrypsin inhibitor' _Abbreviation_common SGCI _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label sgci $sgci stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'all disulfide bound' loop_ _Biological_function 'protease inhibitor' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_sgci _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'Schistocerca gregaria chymotrypsin inhibitor' _Abbreviation_common SGCI _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 35 _Mol_residue_sequence ; EVTCEPGTTFKDKCNTCRCG SDGKSAACTLKACPQ ; loop_ _Residue_seq_code _Residue_label 1 GLU 2 VAL 3 THR 4 CYS 5 GLU 6 PRO 7 GLY 8 THR 9 THR 10 PHE 11 LYS 12 ASP 13 LYS 14 CYS 15 ASN 16 THR 17 CYS 18 ARG 19 CYS 20 GLY 21 SER 22 ASP 23 GLY 24 LYS 25 SER 26 ALA 27 ALA 28 CYS 29 THR 30 LEU 31 LYS 32 ALA 33 CYS 34 PRO 35 GLN stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Organ $sgci 'desert locust' 7010 Eukaryota Metazoa Schistocerca Gregaria brain 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 _Details $sgci 'recombinant technology' 'E. coli' Escherichia coli 'BL21 DE3 pLysS' SGTMCI-pET17b 'Expression of the SGTMCI precursor molecule followed by CNBr cleavage.' 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 $sgci 1.5 mM [U-15N] stop_ save_ ############################ # Computer software used # ############################ save_XEASY _Saveframe_category software _Name XEASY _Version 1.3.6 loop_ _Vendor _Address _Electronic_address 'ETH Zurich' . xeasy@mol.bio.ethz.ch stop_ loop_ _Task 'peak assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-15N HSQC' _Sample_label . save_ save_3D_TOCSY-HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '3D TOCSY-HSQC' _Sample_label . save_ save_3D_NOESY-HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NOESY-HSQC' _Sample_label . save_ save_15N_T1_4 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T1' _Sample_label . save_ save_15N_T2_5 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T2' _Sample_label . save_ save_1H,15N_NOE_6 _Saveframe_category NMR_applied_experiment _Experiment_name '1H,15N NOE' _Sample_label . save_ ####################### # Sample conditions # ####################### save_ex-cond_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6.0 0.2 n/a temperature 300 1 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference _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 water H 1 protons ppm 4.74 internal direct . . . 1.0 DSS N 15 'methyl protons' ppm 0.0 . indirect . . . 0.101329118 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_shift_set_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '1H-15N HSQC' '3D TOCSY-HSQC' '3D NOESY-HSQC' '15N T1' '15N T2' '1H,15N NOE' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $ex-cond_1 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name sgci _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 . 3 THR H H 7.94 0.05 1 2 . 3 THR HA H 4.78 0.05 1 3 . 3 THR HB H 4.02 0.05 2 4 . 3 THR HG2 H 1.15 0.05 1 5 . 3 THR N N 118.95 0.05 1 6 . 4 CYS H H 8.60 0.05 1 7 . 4 CYS HA H 4.63 0.05 1 8 . 4 CYS HB2 H 2.43 0.05 2 9 . 4 CYS HB3 H 2.83 0.05 2 10 . 4 CYS N N 120.78 0.05 1 11 . 5 GLU H H 8.46 0.05 1 12 . 5 GLU HA H 4.70 0.05 1 13 . 5 GLU HB2 H 1.98 0.05 2 14 . 5 GLU HB3 H 2.26 0.05 2 15 . 5 GLU N N 121.14 0.05 1 16 . 7 GLY H H 7.48 0.05 1 17 . 7 GLY HA2 H 3.74 0.05 2 18 . 7 GLY HA3 H 4.24 0.05 2 19 . 7 GLY N N 110.42 0.05 1 20 . 8 THR H H 7.71 0.05 1 21 . 8 THR HA H 4.62 0.05 1 22 . 8 THR N N 111.47 0.05 1 23 . 9 THR H H 8.52 0.05 1 24 . 9 THR HA H 5.52 0.05 1 25 . 9 THR HB H 4.03 0.05 2 26 . 9 THR HG2 H 1.14 0.05 1 27 . 9 THR N N 115.48 0.05 1 28 . 10 PHE H H 8.93 0.05 1 29 . 10 PHE HA H 5.05 0.05 1 30 . 10 PHE HB2 H 3.13 0.05 2 31 . 10 PHE N N 122.05 0.05 1 32 . 11 LYS H H 8.71 0.05 1 33 . 11 LYS HA H 4.76 0.05 1 34 . 11 LYS HB2 H 1.78 0.05 2 35 . 11 LYS N N 120.27 0.05 1 36 . 12 ASP H H 8.08 0.05 1 37 . 12 ASP HA H 4.77 0.05 1 38 . 12 ASP HB2 H 2.47 0.05 2 39 . 12 ASP HB3 H 2.63 0.05 2 40 . 12 ASP N N 123.02 0.05 1 41 . 15 ASN H H 8.51 0.05 1 42 . 15 ASN HA H 4.81 0.05 1 43 . 15 ASN HB2 H 2.59 0.05 2 44 . 15 ASN HB3 H 2.96 0.05 2 45 . 15 ASN N N 122.21 0.05 1 46 . 16 THR H H 8.16 0.05 1 47 . 16 THR HA H 4.54 0.05 1 48 . 16 THR HB H 3.91 0.05 2 49 . 16 THR HG2 H 1.10 0.05 1 50 . 16 THR N N 115.78 0.05 1 51 . 17 CYS H H 8.97 0.05 1 52 . 17 CYS HA H 5.21 0.05 1 53 . 17 CYS HB2 H 1.92 0.39 2 54 . 17 CYS HB3 H 1.09 0.39 2 55 . 17 CYS N N 124.14 0.05 1 56 . 18 ARG H H 8.58 0.05 1 57 . 18 ARG HA H 4.97 0.05 1 58 . 18 ARG HB2 H 1.68 0.05 2 59 . 18 ARG HB3 H 1.80 0.05 2 60 . 18 ARG HG2 H 1.50 0.05 2 61 . 18 ARG N N 121.44 0.05 1 62 . 19 CYS H H 9.51 0.05 1 63 . 19 CYS HA H 4.77 0.05 1 64 . 19 CYS HB2 H 2.93 0.05 2 65 . 19 CYS HB3 H 3.38 0.05 2 66 . 19 CYS N N 128.73 0.05 1 67 . 20 GLY H H 9.18 0.05 1 68 . 20 GLY HA2 H 4.26 0.05 1 69 . 20 GLY HA3 H 4.10 0.16 2 70 . 20 GLY N N 119.04 0.05 1 71 . 22 ASP H H 7.93 0.05 1 72 . 22 ASP HA H 4.53 0.05 1 73 . 22 ASP N N 116.99 0.05 1 74 . 23 GLY H H 7.84 0.05 1 75 . 23 GLY HA2 H 4.03 0.05 2 76 . 23 GLY HA3 H 4.21 0.05 2 77 . 23 GLY N N 108.30 0.05 1 78 . 24 LYS H H 7.93 0.05 1 79 . 24 LYS HA H 5.08 0.05 1 80 . 24 LYS HB2 H 1.50 0.05 2 81 . 24 LYS HB3 H 2.02 0.05 2 82 . 24 LYS HG2 H 1.35 0.05 2 83 . 24 LYS N N 117.95 0.05 1 84 . 26 ALA H H 8.70 0.05 1 85 . 26 ALA HA H 4.76 0.05 1 86 . 26 ALA HB H 1.39 0.05 1 87 . 26 ALA N N 121.59 0.05 1 88 . 27 ALA H H 8.11 0.05 1 89 . 27 ALA HA H 4.76 0.05 1 90 . 27 ALA HB H 1.39 0.05 1 91 . 27 ALA N N 124.51 0.05 1 92 . 29 THR H H 8.50 0.05 1 93 . 29 THR HA H 4.28 0.05 1 94 . 29 THR N N 113.82 0.05 1 95 . 30 LEU H H 8.34 0.05 1 96 . 30 LEU HA H 4.50 0.05 1 97 . 30 LEU HB2 H 1.52 0.05 2 98 . 30 LEU HB3 H 1.68 0.05 2 99 . 30 LEU N N 123.06 0.05 1 100 . 31 LYS H H 8.55 0.05 1 101 . 31 LYS HA H 4.25 0.05 1 102 . 31 LYS HB2 H 1.47 0.05 2 103 . 31 LYS HB3 H 1.77 0.05 2 104 . 31 LYS N N 123.12 0.05 1 stop_ save_ save_T1_relaxation _Saveframe_category T1_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $ex-cond_1 _Spectrometer_frequency_1H 500 _T1_coherence_type Nz _T1_value_units s _Mol_system_component_name sgci _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 3 THR N 1.980 0.012 2 4 CYS N 3.062 0.013 3 5 GLU N 2.081 0.007 4 7 GLY N 2.472 0.028 5 8 THR N 2.697 0.010 6 9 THR N 2.852 0.013 7 10 PHE N 2.343 0.011 8 11 LYS N 2.490 0.015 9 12 ASP N 2.527 0.007 10 15 ASN N 2.325 0.013 11 16 THR N 2.676 0.011 12 17 CYS N 2.385 0.009 13 18 ARG N 2.242 0.009 14 19 CYS N 2.757 0.018 15 20 GLY N 3.105 0.015 16 22 ASP N 3.106 0.013 17 23 GLY N 2.963 0.017 18 24 LYS N 3.182 0.010 19 26 ALA N 1.255 0.013 20 27 ALA N 1.958 0.009 21 29 THR N 1.850 0.027 22 30 LEU N 2.670 0.021 23 31 LYS N 2.487 0.014 stop_ save_ save_15N_T2 _Saveframe_category T2_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $ex-cond_1 _Spectrometer_frequency_1H 500 _T2_coherence_type Nx _T2_value_units s _Mol_system_component_name sgci _Text_data_format . _Text_data . loop_ _T2_ID _Residue_seq_code _Residue_label _Atom_name _T2_value _T2_value_error _Rex_value _Rex_error 1 3 THR N 4.796 0.041 . . 2 4 CYS N 7.127 0.062 . . 3 5 GLU N 5.095 0.024 . . 4 7 GLY N 3.676 0.057 . . 5 8 THR N 5.106 0.027 . . 6 9 THR N 5.202 0.033 . . 7 10 PHE N 3.804 0.026 . . 8 11 LYS N 4.243 0.038 . . 9 12 ASP N 4.835 0.016 . . 10 15 ASN N 5.232 0.044 . . 11 16 THR N 4.812 0.028 . . 12 17 CYS N 4.350 0.021 . . 13 18 ARG N 5.523 0.038 . . 14 19 CYS N 6.663 0.126 . . 15 20 GLY N 11.709 0.117 . . 16 22 ASP N 5.062 0.032 . . 17 23 GLY N 4.644 0.039 . . 18 24 LYS N 5.206 0.024 . . 19 26 ALA N 6.490 0.151 . . 20 27 ALA N 5.950 0.040 . . 21 29 THR N 11.309 0.257 . . 22 30 LEU N 6.899 0.092 . . 23 31 LYS N 5.580 0.041 . . stop_ save_ save_heteronuclear_NOE _Saveframe_category heteronuclear_NOE _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $ex-cond_1 _Spectrometer_frequency_1H 500 _Mol_system_component_name sgci _Atom_one_atom_name N _Atom_two_atom_name H _Heteronuclear_NOE_value_type 'relative intensities' _NOE_reference_value . _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 3 THR 0.231 0.050 4 CYS 0.510 0.050 5 GLU 0.561 0.050 7 GLY 0.456 0.050 8 THR 0.481 0.050 9 THR 0.454 0.050 10 PHE 0.413 0.050 11 LYS 0.576 0.050 12 ASP 0.454 0.050 15 ASN 0.524 0.050 16 THR 0.413 0.050 17 CYS 0.432 0.050 18 ARG 0.393 0.050 19 CYS 0.484 0.050 20 GLY 0.483 0.050 22 ASP 0.454 0.050 23 GLY 0.432 0.050 24 LYS 0.398 0.050 26 ALA 0.426 0.050 27 ALA 0.404 0.050 29 THR 0.455 0.050 30 LEU 0.444 0.050 31 LYS 0.392 0.050 stop_ save_