data_6881 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H, 13C and 15N chemical shift assignments of Schistocerca gregaria chymotrypsin inhibitor complexed with bovine chymotrypsin ; _BMRB_accession_number 6881 _BMRB_flat_file_name bmr6881.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" 18 "13C chemical shifts" 33 "15N chemical shifts" 18 "T1 relaxation values" 18 "T2 relaxation values" 18 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' 6880 '1H and 15N chemical shift assignments of Schistocerca gregaria chymotrypsin inhibitor at pH=6.0' stop_ 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 'protease inhibitor' Schistocerca SGCI stop_ save_ ################################## # Molecular system description # ################################## save_system_SGCI _Saveframe_category molecular_system _Mol_system_name 'Schistocerca gregaria chymotrypsin inhibitor complex with bovine alpha-chymotrypsin' _Abbreviation_common SGCI _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label sgci $sgci 'bovine alpha-chymotrypsin' $bovine_alpha_chymotrypsin stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state dimer _System_paramagnetic no _System_thiol_state 'all disulfide bound' loop_ _Biological_function protease '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_ save_bovine_alpha_chymotrypsin _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'bovine alpha-chymotrypsin' _Abbreviation_common 'bovine alpha-chymotrypsin' _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . _Residue_count 241 _Mol_residue_sequence ; CGVPAIQPVLSGLIVNGEEA VPGSWPWQVSLQDKTGFHFC GGSLINENWVVTAAHCGVTT SDVVVAGEFDQGSSSEKIQK LKIAKVFKNSKYNSLTINND ITLLKLSTAASFSQTVSAVC LPSASDDFAAGTTCVTTGWG LTRYTNTPDRLQQASLPLLS NTNCKKYWGTKIKDAMICAG ASGVSSCMGDSGGPLVCKKN GAWTLVGIVSWGSSTCSTST PGVYARVTALVNWVQQTLAA N ; loop_ _Residue_seq_code _Residue_label 1 CYS 2 GLY 3 VAL 4 PRO 5 ALA 6 ILE 7 GLN 8 PRO 9 VAL 10 LEU 11 SER 12 GLY 13 LEU 14 ILE 15 VAL 16 ASN 17 GLY 18 GLU 19 GLU 20 ALA 21 VAL 22 PRO 23 GLY 24 SER 25 TRP 26 PRO 27 TRP 28 GLN 29 VAL 30 SER 31 LEU 32 GLN 33 ASP 34 LYS 35 THR 36 GLY 37 PHE 38 HIS 39 PHE 40 CYS 41 GLY 42 GLY 43 SER 44 LEU 45 ILE 46 ASN 47 GLU 48 ASN 49 TRP 50 VAL 51 VAL 52 THR 53 ALA 54 ALA 55 HIS 56 CYS 57 GLY 58 VAL 59 THR 60 THR 61 SER 62 ASP 63 VAL 64 VAL 65 VAL 66 ALA 67 GLY 68 GLU 69 PHE 70 ASP 71 GLN 72 GLY 73 SER 74 SER 75 SER 76 GLU 77 LYS 78 ILE 79 GLN 80 LYS 81 LEU 82 LYS 83 ILE 84 ALA 85 LYS 86 VAL 87 PHE 88 LYS 89 ASN 90 SER 91 LYS 92 TYR 93 ASN 94 SER 95 LEU 96 THR 97 ILE 98 ASN 99 ASN 100 ASP 101 ILE 102 THR 103 LEU 104 LEU 105 LYS 106 LEU 107 SER 108 THR 109 ALA 110 ALA 111 SER 112 PHE 113 SER 114 GLN 115 THR 116 VAL 117 SER 118 ALA 119 VAL 120 CYS 121 LEU 122 PRO 123 SER 124 ALA 125 SER 126 ASP 127 ASP 128 PHE 129 ALA 130 ALA 131 GLY 132 THR 133 THR 134 CYS 135 VAL 136 THR 137 THR 138 GLY 139 TRP 140 GLY 141 LEU 142 THR 143 ARG 144 TYR 145 THR 146 ASN 147 THR 148 PRO 149 ASP 150 ARG 151 LEU 152 GLN 153 GLN 154 ALA 155 SER 156 LEU 157 PRO 158 LEU 159 LEU 160 SER 161 ASN 162 THR 163 ASN 164 CYS 165 LYS 166 LYS 167 TYR 168 TRP 169 GLY 170 THR 171 LYS 172 ILE 173 LYS 174 ASP 175 ALA 176 MET 177 ILE 178 CYS 179 ALA 180 GLY 181 ALA 182 SER 183 GLY 184 VAL 185 SER 186 SER 187 CYS 188 MET 189 GLY 190 ASP 191 SER 192 GLY 193 GLY 194 PRO 195 LEU 196 VAL 197 CYS 198 LYS 199 LYS 200 ASN 201 GLY 202 ALA 203 TRP 204 THR 205 LEU 206 VAL 207 GLY 208 ILE 209 VAL 210 SER 211 TRP 212 GLY 213 SER 214 SER 215 THR 216 CYS 217 SER 218 THR 219 SER 220 THR 221 PRO 222 GLY 223 VAL 224 TYR 225 ALA 226 ARG 227 VAL 228 THR 229 ALA 230 LEU 231 VAL 232 ASN 233 TRP 234 VAL 235 GLN 236 GLN 237 THR 238 LEU 239 ALA 240 ALA 241 ASN 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 $bovine_alpha_chymotrypsin Cow 9913 Eukaryota Metazoa Bos taurus pancreas 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' . . 'BL21 DE3 pLysS' SGTMCI-pET17b 'Expression of the SGTMCI precursor molecule followed by CNBr cleavage.' $bovine_alpha_chymotrypsin 'purchased from commercial source' . . . . . 'purchased from Sigma.' 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 0.68 mM [U-15N] $bovine_alpha_chymotrypsin 0.85 mM . stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $sgci 0.68 mM '[U-13C; U-15N]' $bovine_alpha_chymotrypsin 0.85 mM . 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_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details . save_ save_NMR_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model Inova _Field_strength 600 _Details . save_ save_NMR_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model Inova _Field_strength 900 _Details . save_ ############################# # NMR applied experiments # ############################# save_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-15N HSQC' _Sample_label . save_ save_15N_T1_2 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T1' _Sample_label . save_ save_15N_T2_3 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T2' _Sample_label . save_ save_1H,15N_NOE_4 _Saveframe_category NMR_applied_experiment _Experiment_name '1H,15N NOE' _Sample_label . save_ save_HNCA_5 _Saveframe_category NMR_applied_experiment _Experiment_name HNCA _Sample_label . save_ save_HNCOCA_6 _Saveframe_category NMR_applied_experiment _Experiment_name HNCOCA _Sample_label . save_ save_HNCACB_7 _Saveframe_category NMR_applied_experiment _Experiment_name HNCACB _Sample_label . save_ save_CBCACONH_8 _Saveframe_category NMR_applied_experiment _Experiment_name CBCACONH _Sample_label . save_ save_NMR_spec_expt__0_1 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-15N HSQC' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_2 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T1' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_3 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T2' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_4 _Saveframe_category NMR_applied_experiment _Experiment_name '1H,15N NOE' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_5 _Saveframe_category NMR_applied_experiment _Experiment_name HNCA _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_6 _Saveframe_category NMR_applied_experiment _Experiment_name HNCOCA _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_7 _Saveframe_category NMR_applied_experiment _Experiment_name HNCACB _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_8 _Saveframe_category NMR_applied_experiment _Experiment_name CBCACONH _BMRB_pulse_sequence_accession_number . _Details . 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 na 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 DSS C 13 'methyl protons' ppm 0.0 . indirect . . . 0.251449530 water H 1 protons ppm 4.74 internal direct . . . 1.000000000 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' '15N T1' '15N T2' '1H,15N NOE' HNCA HNCOCA HNCACB CBCACONH 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 . 7 GLY CA C 46.12 0.06 1 2 . 7 GLY H H 7.28 0.05 1 3 . 7 GLY N N 110.13 0.05 1 4 . 8 THR CA C 62.18 0.05 1 5 . 8 THR CB C 72.19 0.05 1 6 . 8 THR H H 7.67 0.02 1 7 . 8 THR N N 111.28 0.05 1 8 . 9 THR CA C 61.47 0.06 1 9 . 9 THR CB C 69.59 0.62 1 10 . 9 THR H H 8.55 0.05 1 11 . 9 THR N N 117.05 0.05 1 12 . 10 PHE CA C 55.66 0.05 1 13 . 10 PHE CB C 40.99 0.04 1 14 . 10 PHE H H 8.98 0.03 1 15 . 10 PHE N N 123.16 0.05 1 16 . 11 LYS CA C 55.17 0.05 1 17 . 11 LYS CB C 33.68 0.05 1 18 . 11 LYS H H 8.77 0.05 1 19 . 11 LYS N N 119.99 0.05 1 20 . 12 ASP CA C 52.95 0.02 1 21 . 12 ASP CB C 41.41 0.05 1 22 . 12 ASP H H 8.19 0.05 1 23 . 12 ASP N N 123.07 0.05 1 24 . 13 LYS CA C 58.83 0.05 1 25 . 13 LYS CB C 30.11 0.05 1 26 . 13 LYS H H 9.38 0.05 1 27 . 13 LYS N N 123.71 0.02 1 28 . 14 CYS CA C 59.38 0.05 1 29 . 14 CYS CB C 35.85 0.05 1 30 . 14 CYS H H 8.81 0.05 1 31 . 14 CYS N N 120.28 0.05 1 32 . 15 ASN CA C 53.67 0.12 1 33 . 15 ASN CB C 41.55 0.05 1 34 . 15 ASN H H 8.32 0.05 1 35 . 15 ASN N N 122.99 0.05 1 36 . 16 THR CA C 62.37 0.61 1 37 . 16 THR CB C 69.77 0.29 1 38 . 16 THR H H 8.10 0.05 1 39 . 16 THR N N 116.56 0.19 1 40 . 17 CYS CA C 54.92 0.05 1 41 . 17 CYS CB C 50.05 0.05 1 42 . 17 CYS H H 8.93 0.05 1 43 . 17 CYS N N 124.81 0.03 1 44 . 18 ARG CA C 54.62 0.05 1 45 . 18 ARG CB C 33.11 0.05 1 46 . 18 ARG H H 8.95 0.05 1 47 . 18 ARG N N 119.43 0.05 1 48 . 19 CYS CA C 56.60 0.02 1 49 . 19 CYS H H 9.56 0.05 1 50 . 19 CYS CB C 41.97 0.05 1 51 . 19 CYS N N 126.08 0.05 1 52 . 20 GLY CA C 45.42 0.03 1 53 . 20 GLY H H 9.36 0.05 1 54 . 20 GLY N N 119.46 0.05 1 55 . 21 SER CA C 61.21 0.05 1 56 . 21 SER CB C 62.95 0.05 1 57 . 21 SER H H 8.89 0.05 1 58 . 21 SER N N 116.60 0.05 1 59 . 22 ASP CA C 53.17 0.05 1 60 . 22 ASP CB C 40.96 0.05 1 61 . 22 ASP H H 8.00 0.05 1 62 . 22 ASP N N 117.03 0.05 1 63 . 23 GLY CA C 47.05 0.05 1 64 . 23 GLY H H 7.79 0.05 1 65 . 23 GLY N N 107.91 0.05 1 66 . 24 LYS CA C 55.24 0.05 1 67 . 24 LYS CB C 33.82 0.05 1 68 . 24 LYS H H 8.00 0.05 1 69 . 24 LYS N N 117.66 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 7 GLY N 1.436 0.004 2 8 THR N 1.514 0.012 3 9 THR N 1.466 0.002 4 10 PHE N 1.515 0.003 5 11 LYS N 1.239 0.002 6 12 ASP N 1.440 0.003 7 13 LYS N 1.160 0.005 8 14 CYS N 1.471 0.006 9 15 ASN N 1.582 0.003 10 16 THR N 1.486 0.003 11 17 CYS N 1.513 0.004 12 18 ARG N 1.480 0.007 13 19 CYS N 1.518 0.011 14 20 GLY N 1.585 0.006 15 21 SER N 1.442 0.001 16 22 ASP N 1.465 0.002 17 23 GLY N 1.401 0.002 18 24 LYS N 1.459 0.006 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 7 GLY N 15.720 0.040 . . 2 8 THR N 23.669 0.179 . . 3 9 THR N 17.099 0.025 . . 4 10 PHE N 17.659 0.036 . . 5 11 LYS N 15.210 0.023 . . 6 12 ASP N 16.348 0.025 . . 7 13 LYS N 17.361 0.058 . . 8 14 CYS N 15.390 0.048 . . 9 15 ASN N 18.029 0.025 . . 10 16 THR N 16.540 0.026 . . 11 17 CYS N 14.192 0.030 . . 12 18 ARG N 16.695 0.066 . . 13 19 CYS N 19.175 0.112 . . 14 20 GLY N 19.292 0.062 . . 15 21 SER N 16.526 0.011 . . 16 22 ASP N 17.560 0.020 . . 17 23 GLY N 17.512 0.018 . . 18 24 LYS N 15.298 0.051 . . 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 7 GLY 0.542 0.050 8 THR 0.647 0.050 9 THR 0.516 0.050 10 PHE 0.718 0.050 11 LYS 0.793 0.050 12 ASP 1.203 0.050 13 LYS 0.875 0.050 14 CYS 0.793 0.050 15 ASN 0.586 0.050 16 THR -0.440 0.050 17 CYS 0.608 0.050 18 ARG 0.890 0.050 19 CYS 0.899 0.050 20 GLY 0.690 0.050 21 SER 0.717 0.050 22 ASP 0.754 0.050 23 GLY 0.752 0.050 24 LYS 0.340 0.050 stop_ save_