data_4351 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; A 30-residue Fragment of the Carp Granulin-1 Protein Folds into a Stack of two Beta-hairpins Similar to that found in the Native Protein ; _BMRB_accession_number 4351 _BMRB_flat_file_name bmr4351.str _Entry_type update _Submission_date 1999-06-03 _Accession_date 1999-06-04 _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 Vranken Wim F. . 2 Chen Z. G. . 3 Xu Ping . . 4 James Susan . . 5 Bennett Hugh P.J. . 6 Ni Feng . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 coupling_constants 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 151 "13C chemical shifts" 53 "coupling constants" 5 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2000-12-15 original author 'original release' 2001-03-15 update author '13C chemical shifts added' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; A 30-residue Fragment of the Carp Granulin-1 Protein Folds into a Stack of two Beta-hairpins Similar to that found in the Native Protein ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code 99351641 _PubMed_ID 10424355 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Vranken Wim F. . 2 Chen Z. G. . 3 Xu Ping . . 4 James Susan . . 5 Bennett Hugh P.J. . 6 Ni Feng . . stop_ _Journal_abbreviation 'J. Pept. Res.' _Journal_volume 53 _Journal_issue 5 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 590 _Page_last 597 _Year 1999 _Details . loop_ _Keyword 'granulin repeat' 'hairpin stack fold' 'NMR structure' stop_ save_ ################################## # Molecular system description # ################################## save_system_GRN1_CYPCA _Saveframe_category molecular_system _Mol_system_name 'granulin N-terminal peptide' _Abbreviation_common 'GRN1 CYPCA' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'GRN1 CYPCA' $GRN1_CYPCA stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'not reported' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_GRN1_CYPCA _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common granulin _Name_variant 'carp granulin 1' _Abbreviation_common 'GRN1 CYPCA' _Molecular_mass . _Mol_thiol_state 'not reported' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 30 _Mol_residue_sequence ; VIHCDAATICPDGTTCSLSP YGVWYCSPFS ; loop_ _Residue_seq_code _Residue_label 1 VAL 2 ILE 3 HIS 4 CYS 5 ASP 6 ALA 7 ALA 8 THR 9 ILE 10 CYS 11 PRO 12 ASP 13 GLY 14 THR 15 THR 16 CYS 17 SER 18 LEU 19 SER 20 PRO 21 TYR 22 GLY 23 VAL 24 TRP 25 TYR 26 CYS 27 SER 28 PRO 29 PHE 30 SER stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-03-16 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value PDB 1I8X "Semi-Automatic Structure Determination Of The Cg1 1-30 Peptide Based On Aria" 100.00 30 100.00 100.00 4.16e-12 PDB 1I8Y "Semi-Automatic Structure Determination Of The Cg1 3-30 Peptide Based On Aria" 93.33 28 100.00 100.00 8.81e-11 PDB 1QGM "The Solution Structure Of A 30 Residue Amino-Terminal Domain Of The Carp Granulin-1 Protein." 100.00 30 100.00 100.00 4.16e-12 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Organ _Gene_mnemonic $GRN1_CYPCA carp 7962 Eukaryota Metazoa Cyprinus carpio liver GRN1_CYPCA 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 $GRN1_CYPCA 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_water_sample _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $GRN1_CYPCA 0.54 mM . stop_ save_ ############################ # Computer software used # ############################ save_XWIN-NMR _Saveframe_category software _Name XWIN-NMR _Version . loop_ _Task 'Spectrum processing' stop_ _Details . save_ save_PRONTO _Saveframe_category software _Name PRONTO _Version . loop_ _Task ; Assignment of spectra and keeping record of NOE contacts ; stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 500 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 800 _Details . save_ ############################# # NMR applied experiments # ############################# save_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name TOCSY _Sample_label $water_sample save_ save_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name NOESY _Sample_label $water_sample save_ save_TOCSY_spinlock_with_MLEV-17_3 _Saveframe_category NMR_applied_experiment _Experiment_name 'TOCSY spinlock with MLEV-17' _Sample_label $water_sample save_ save_NOESY_using_water_flipback_4 _Saveframe_category NMR_applied_experiment _Experiment_name 'NOESY using water flipback' _Sample_label $water_sample save_ save_Water_suppression_with_WATERGATE_5 _Saveframe_category NMR_applied_experiment _Experiment_name 'Water suppression with WATERGATE' _Sample_label $water_sample save_ ####################### # Sample conditions # ####################### save_standard _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.02 0.01 M pH 4.5 0.1 n/a pressure 1 . atm temperature 288.0 0.2 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_citation_label _Correction_value_citation_label . C 13 . . . . . . . . $entry_citation $entry_citation DSS H 1 'methyl protons' ppm 0.0 internal direct . . . $entry_citation $entry_citation 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_ _Sample_label $water_sample stop_ _Sample_conditions_label $standard _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name 'GRN1 CYPCA' _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 VAL CA C 61.358 0.1 1 2 . 1 VAL HA H 3.890 0.02 1 3 . 1 VAL CB C 27.267 0.1 1 4 . 1 VAL HB H 2.080 0.02 1 5 . 1 VAL HG2 H 0.740 0.02 1 6 . 1 VAL HG1 H 0.900 0.02 1 7 . 2 ILE H H 8.930 0.02 1 8 . 2 ILE CA C 59.834 0.1 1 9 . 2 ILE HA H 4.390 0.02 1 10 . 2 ILE CB C 40.160 0.1 1 11 . 2 ILE HB H 1.660 0.02 1 12 . 2 ILE HG13 H 1.410 0.02 1 13 . 2 ILE HG12 H 1.410 0.02 1 14 . 2 ILE HD1 H 1.050 0.02 1 15 . 2 ILE HG2 H 0.860 0.02 1 16 . 3 HIS H H 9.110 0.02 1 17 . 3 HIS CA C 56.358 0.1 1 18 . 3 HIS HA H 4.790 0.02 1 19 . 3 HIS CB C 29.955 0.1 1 20 . 3 HIS HB3 H 3.080 0.02 1 21 . 3 HIS HB2 H 3.080 0.02 1 22 . 3 HIS HD2 H 7.300 0.02 1 23 . 3 HIS HE1 H 8.640 0.02 1 24 . 5 ASP CA C 52.695 0.1 1 25 . 5 ASP HA H 4.260 0.02 1 26 . 5 ASP CB C 40.540 0.1 1 27 . 5 ASP HB3 H 3.160 0.02 2 28 . 5 ASP HB2 H 2.940 0.02 2 29 . 6 ALA H H 8.410 0.02 1 30 . 6 ALA CA C 54.587 0.1 1 31 . 6 ALA HA H 4.060 0.02 1 32 . 6 ALA CB C 18.398 0.1 1 33 . 6 ALA HB H 1.400 0.02 1 34 . 7 ALA H H 7.850 0.02 1 35 . 7 ALA CA C 51.891 0.1 1 36 . 7 ALA HA H 4.530 0.02 1 37 . 7 ALA CB C 20.836 0.1 1 38 . 7 ALA HB H 1.450 0.02 1 39 . 8 THR H H 7.900 0.02 1 40 . 8 THR CA C 63.294 0.1 1 41 . 8 THR HA H 4.320 0.02 1 42 . 8 THR CB C 69.630 0.1 1 43 . 8 THR HB H 3.630 0.02 1 44 . 8 THR HG2 H 1.070 0.02 1 45 . 9 ILE H H 8.560 0.02 1 46 . 9 ILE CA C 59.675 0.1 1 47 . 9 ILE HA H 4.630 0.02 1 48 . 9 ILE CB C 39.603 0.1 1 49 . 9 ILE HB H 1.550 0.02 1 50 . 9 ILE HG13 H 1.320 0.02 1 51 . 9 ILE HG12 H 1.320 0.02 1 52 . 9 ILE HD1 H 0.720 0.02 1 53 . 9 ILE HG2 H 0.530 0.02 1 54 . 10 CYS H H 8.950 0.02 1 55 . 10 CYS HA H 5.250 0.02 1 56 . 10 CYS CB C 38.170 0.1 1 57 . 10 CYS HB3 H 3.670 0.02 2 58 . 10 CYS HB2 H 2.090 0.02 2 59 . 11 PRO CA C 62.181 0.1 1 60 . 11 PRO HA H 4.450 0.02 1 61 . 11 PRO CB C 32.538 0.1 1 62 . 11 PRO HB3 H 2.300 0.02 2 63 . 11 PRO HB2 H 1.940 0.02 2 64 . 11 PRO HG3 H 2.010 0.02 2 65 . 11 PRO HG2 H 1.940 0.02 2 66 . 11 PRO HD3 H 3.850 0.02 1 67 . 11 PRO HD2 H 3.760 0.02 1 68 . 12 ASP H H 8.730 0.02 1 69 . 12 ASP CA C 56.112 0.1 1 70 . 12 ASP HA H 4.430 0.02 1 71 . 12 ASP CB C 40.430 0.1 1 72 . 12 ASP HB3 H 2.740 0.02 1 73 . 12 ASP HB2 H 2.600 0.02 1 74 . 13 GLY H H 9.030 0.02 1 75 . 13 GLY CA C 44.937 0.1 1 76 . 13 GLY HA3 H 4.210 0.02 2 77 . 13 GLY HA2 H 3.590 0.02 2 78 . 14 THR H H 7.740 0.02 1 79 . 14 THR CA C 59.973 0.1 1 80 . 14 THR HA H 4.950 0.02 1 81 . 14 THR CB C 72.442 0.1 1 82 . 14 THR HB H 3.800 0.02 1 83 . 14 THR HG2 H 0.890 0.02 1 84 . 15 THR H H 8.810 0.02 1 85 . 15 THR CA C 59.988 0.1 1 86 . 15 THR HA H 4.560 0.02 1 87 . 15 THR CB C 71.255 0.1 1 88 . 15 THR HB H 3.900 0.02 1 89 . 15 THR HG2 H 1.100 0.02 1 90 . 16 CYS H H 8.600 0.02 1 91 . 16 CYS CA C 57.368 0.1 1 92 . 16 CYS HA H 4.850 0.02 1 93 . 16 CYS CB C 41.357 0.1 1 94 . 16 CYS HB3 H 3.040 0.02 2 95 . 16 CYS HB2 H 2.940 0.02 2 96 . 17 SER H H 9.390 0.02 1 97 . 17 SER CA C 57.532 0.1 1 98 . 17 SER HA H 4.820 0.02 1 99 . 17 SER CB C 65.496 0.1 1 100 . 17 SER HB3 H 3.430 0.02 2 101 . 17 SER HB2 H 2.800 0.02 2 102 . 18 LEU H H 8.470 0.02 1 103 . 18 LEU CA C 53.630 0.1 1 104 . 18 LEU HA H 4.120 0.02 1 105 . 18 LEU CB C 42.587 0.1 1 106 . 18 LEU HB3 H -0.315 0.02 2 107 . 18 LEU HB2 H 1.210 0.02 2 108 . 18 LEU HG H 0.920 0.02 1 109 . 18 LEU HD1 H 0.190 0.02 1 110 . 18 LEU HD2 H -0.310 0.02 1 111 . 19 SER H H 9.230 0.02 1 112 . 19 SER CA C 56.597 0.1 1 113 . 19 SER HA H 4.950 0.02 1 114 . 19 SER CB C 63.392 0.1 1 115 . 19 SER HB3 H 4.480 0.02 2 116 . 19 SER HB2 H 4.150 0.02 2 117 . 20 PRO CA C 64.322 0.1 1 118 . 20 PRO HA H 4.310 0.02 1 119 . 20 PRO CB C 31.479 0.1 1 120 . 20 PRO HB3 H 2.240 0.02 1 121 . 20 PRO HB2 H 1.260 0.02 1 122 . 20 PRO HG3 H 1.950 0.02 2 123 . 20 PRO HG2 H 1.880 0.02 2 124 . 20 PRO HD3 H 3.980 0.02 1 125 . 20 PRO HD2 H 3.660 0.02 1 126 . 21 TYR H H 7.370 0.02 1 127 . 21 TYR CA C 56.240 0.1 1 128 . 21 TYR HA H 4.650 0.02 1 129 . 21 TYR CB C 37.777 0.1 1 130 . 21 TYR HB3 H 3.410 0.02 2 131 . 21 TYR HB2 H 2.550 0.02 2 132 . 21 TYR HD1 H 7.110 0.02 1 133 . 21 TYR HE1 H 6.850 0.02 1 134 . 21 TYR HE2 H 6.850 0.02 1 135 . 21 TYR HD2 H 7.110 0.02 1 136 . 22 GLY H H 8.000 0.02 1 137 . 22 GLY CA C 46.084 0.1 1 138 . 22 GLY HA3 H 4.050 0.02 2 139 . 22 GLY HA2 H 3.420 0.02 2 140 . 23 VAL H H 7.190 0.02 1 141 . 23 VAL CA C 60.516 0.1 1 142 . 23 VAL HA H 4.230 0.02 1 143 . 23 VAL CB C 27.540 0.1 1 144 . 23 VAL HB H 1.940 0.02 1 145 . 23 VAL HG2 H 0.840 0.02 1 146 . 23 VAL HG1 H 0.990 0.02 1 147 . 24 TRP H H 8.670 0.02 1 148 . 24 TRP CA C 57.209 0.1 1 149 . 24 TRP HA H 5.280 0.02 1 150 . 24 TRP CB C 30.510 0.1 1 151 . 24 TRP HB3 H 3.090 0.02 1 152 . 24 TRP HB2 H 3.090 0.02 1 153 . 24 TRP HD1 H 7.330 0.02 1 154 . 24 TRP HE1 H 10.070 0.02 1 155 . 24 TRP HZ2 H 7.470 0.02 1 156 . 24 TRP HH2 H 7.200 0.02 1 157 . 24 TRP HZ3 H 6.790 0.02 1 158 . 24 TRP HE3 H 7.440 0.02 1 159 . 25 TYR H H 9.840 0.02 1 160 . 25 TYR CA C 55.784 0.1 1 161 . 25 TYR HA H 5.110 0.02 1 162 . 25 TYR HB3 H 3.050 0.02 1 163 . 25 TYR HB2 H 3.050 0.02 1 164 . 25 TYR HD1 H 7.130 0.02 1 165 . 25 TYR HE1 H 6.570 0.02 1 166 . 25 TYR HE2 H 6.570 0.02 1 167 . 25 TYR HD2 H 7.130 0.02 1 168 . 26 CYS H H 8.710 0.02 1 169 . 26 CYS HA H 5.260 0.02 1 170 . 26 CYS CB C 38.465 0.1 1 171 . 26 CYS HB3 H 3.130 0.02 2 172 . 26 CYS HB2 H 2.850 0.02 2 173 . 27 SER H H 9.280 0.02 1 174 . 27 SER CA C 55.349 0.1 1 175 . 27 SER HA H 5.010 0.02 1 176 . 27 SER CB C 64.503 0.1 1 177 . 27 SER HB3 H 3.830 0.02 2 178 . 27 SER HB2 H 3.730 0.02 2 179 . 28 PRO CA C 63.215 0.1 1 180 . 28 PRO HA H 4.610 0.02 1 181 . 28 PRO CB C 32.076 0.1 1 182 . 28 PRO HB3 H 2.310 0.02 2 183 . 28 PRO HB2 H 2.010 0.02 2 184 . 28 PRO HG3 H 2.010 0.02 2 185 . 28 PRO HG2 H 1.940 0.02 2 186 . 28 PRO HD3 H 3.990 0.02 2 187 . 28 PRO HD2 H 3.830 0.02 2 188 . 29 PHE H H 8.130 0.02 1 189 . 29 PHE CA C 57.644 0.1 1 190 . 29 PHE HA H 4.660 0.02 1 191 . 29 PHE CB C 39.815 0.1 1 192 . 29 PHE HB3 H 3.070 0.02 2 193 . 29 PHE HB2 H 3.020 0.02 2 194 . 29 PHE HD1 H 7.210 0.02 1 195 . 29 PHE HE1 H 7.300 0.02 1 196 . 29 PHE HZ H 7.230 0.02 1 197 . 29 PHE HE2 H 7.300 0.02 1 198 . 29 PHE HD2 H 7.210 0.02 1 199 . 30 SER H H 8.180 0.02 1 200 . 30 SER CA C 59.702 0.1 1 201 . 30 SER HA H 4.310 0.02 1 202 . 30 SER CB C 64.922 0.1 1 203 . 30 SER HB3 H 3.860 0.02 2 204 . 30 SER HB2 H 3.800 0.02 2 stop_ save_ ######################## # Coupling constants # ######################## save_J_values _Saveframe_category coupling_constants _Details . loop_ _Sample_label $water_sample stop_ _Sample_conditions_label $standard _Spectrometer_frequency_1H . _Mol_system_component_name 'GRN1 CYPCA' _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 7 ALA H 7 ALA HA 9.9 . . 1.0 2 3JHNHA 15 THR H 15 THR HA 9.9 . . 1.0 3 3JHNHA 21 TYR H 21 TYR HA 9.1 . . 1.0 4 3JHNHA 23 VAL H 23 VAL HA 8.6 . . 1.0 5 3JHNHA 29 PHE H 29 PHE HA 9.9 . . 1.0 stop_ save_